processing of kaolin-based microfiltration...

Journal of the Korean Ceramic Society

Vol. 50, No. 5, pp. 341~347, 2013.

− 341 −

http://dx.doi.org/10.4191/kcers.2013.50.5.341

†Corresponding author : Young-Wook Kim

E-mail : [email protected]

Tel : +82-2-6490-2407 Fax : +82-2-6490- 2404

Processing of Kaolin-Based Microfiltration Membranes

Jung-Hye Eom, Young-Wook Kim†, and In-Hyuck Song*

Functional Ceramics Laboratory, Department of Materials Science and Engineering,

The University of Seoul, 90 Jeonnong-dong, Dongdaemun-ku, Seoul 130-743, Korea

*Engineering Ceramics Group, Korea Institute of Materials Science, 531 Changwondaero, Changwon, Gyeongnam 641-831, Korea

(Received August 19, 2013; Revised September 11, 2013; Accepted September 12, 2013)

ABSTRACT

Kaolin-based membranes with a pore size of 0.30-0.40 µm were successfully prepared by a simple pressing route using low-cost

starting materials, kaolin and sodium borate. The prepared green bodies were sintered at different temperatures ranging

between 900 and 1200oC. The sintered membranes were characterized by X-ray diffraction, mercury porosimetry, scanning elec-

tron microscopy, and capillary flowmetry. It was observed that the porosity decreased with an increase in both the sintering tem-

perature and the sodium borate content, whereas the flexural strength increased with an increase in both the sintering

temperature and the sodium borate content. The air flow rate decreased with an increase in the sodium borate content. The typ-

ical porosity, flexural strength, and specific flow rate of the kaolin-based membrane sintered with 5 wt% sodium borate at 1100oC

were 37%, 19 MPa, and 1 × 10−3 L/min/cm2, respectively, at a p of 30 psi.

Key words : Membranes, Clay, Processing, Porosity, Permeability

1. Introduction

ompared to polymeric membranes, ceramic membranes

have many potential advantages, such as excellent ther-

mal, chemical and mechanical stability, longer life times,

and simple cleaning processes.1-8) These properties make the

ceramic membranes suitable for many applications, such as

water purification, the removal of oil from oil-contaminated

water, the clarification and sterilization of beverages, the

concentrating of proteins in the food and dairy industries,

and the recovery of lignin in the paper industries.9,10)

Generally, the majority of ceramic membranes have been

prepared from alumina (Al2O

3), zirconia (ZrO

2), titania

(TiO2), and silica (SiO

2),11-15) and many research works have

been carried out with those membranes or their composites.

However, the application of ceramic membranes is consider-

ably limited by the high cost of the above materials and

related processing steps. Thus, many researchers have

focused on the development of new types of cost-effective

inorganic membranes, such as zeolite membranes16) and

natural mineral-based ceramic membranes.17-22) Kaolin is

often used as one of the raw materials in the synthesis of

zeolite or mullite membranes.23-25)Zeolite hydroxysodalite

was synthesized by a hydrothermal method using natural

kaolin.23) Abbasi et al.24) processed mullite and mullite-alu-

mina ceramic microfiltration membranes synthesized from

kaolin and α-alumina for the treatment of oily wastewater.

Chen et al.25) processed macroporous mullite membrane sup-

ports through an in situ reaction sintering using kaolin

combined with Al sources, Al(OH)3 and AlF

3.

Kaolin can be a good material with which to fabricate low-

cost ceramic membranes. Many researchers have reported

the use of kaolin as a starting material with other additives

for membrane applications.17-22) Bouzerara et al.20) fabricated

ceramic membrane supports from kaolin-doloma mixtures.

The manufactured membrane supports are mainly com-

posed of mullite, cordierite and anorthite phases, and their

tensile strengths ranged from 6 to 15 MPa, which was likely

acceptable as a support for microfiltration and ultrafiltra-

tion applications. Nandi et al.26) fabricated ceramic microfil-

tration membranes using kaolin, quartz, calcium carbonate,

sodium carbonate, boric acid, and sodium metasilicate as

raw materials, characterizing the feasibility of the mem-

branes for juice processing applications. The results con-

firmed the greater applicability of low-cost ceramic membranes

for beverage processing applications, in contrast to the widely

applicable polymeric membranes. Vasanth et al.27) also pro-

cessed low-cost ceramic membrane supports using kaolin,

quartz, and calcium carbonate, sodium carbonate, boric

acid, sodium metasilicate as raw materials by uniaxial dry

compaction. The prepared supports offer good flexural

strength (22 to 31 MPa) and chemical stability (< 2% weight

loss in acidic media and no weight loss in basic media). Khe-

makhem et al.28) prepared microfiltration membranes from

Tunisian clay materials. The membranes consisted of a clay

skin layer prepared by a slip-casting method deposited on a

silty marls support. They demonstrated the possibility of

C

342 Journal of the Korean Ceramic Society - Jung-Hye Eom et al. Vol. 50, No. 5

the application of the membranes for cuttlefish effluent clar-

ification. The above results17-22,28) suggest that low-cost

ceramic membranes prepared from natural materials are

likely readily applicable to areas such as beverage process-

ing and wastewater treatment.

Studies using sodium borate (Na2B

4O

7·10H

2O) as a bond-

ing phase for kaolin have not yet been reported. Sodium

borate melts at a temperature below 750oC. The low melting

temperature suggests the possibility of the low-temperature

processing of kaolin-based membranes. In the present work,

ceramic membranes were fabricated by a simple uniaxial

pressing route using kaolin and sodium borate as an addi-

tive. The effects of the additive content and the sintering

temperature on the porosity and flexural strength of the

kaolin-based ceramic membranes were investigated. In

addition, the pore size distribution and permeability of a

number of selected membranes were characterized.

2. Experimental Procedure

Commercially available kaolin (Al2O

3· 2SiO

2· 2H

2O, extra

pure, Samchun Pure Chemical Co. Ltd., Pyongtaek, Korea)

and sodium borate (Na2B

4O

7· 10H

2O, first grade, Shinyo

Pure Chemical Co. Ltd., Hyogo, Japan) powders were used

as the starting materials. Sodium borate was added to

increase the mechanical strength of the kaolin-based mem-

branes.29) Five batches of powder mixtures were prepared

with varying sodium borate contents: 0, 1, 2, 3, and 5 wt%

(see Table 1). All batches were mixed separately in a

polypropylene jar for 3 h using distilled water and Al2O

3

grinding balls to make the raw materials homogeneous.

Polyethylene glycol was added as a binder. The milled

slurry was dried at 100oC for 24 h and was uniaxially

pressed at a pressure of 50 MPa. The compacts were sin-

tered at 900, 1000, 1100, and 1200oC for 2 h in air.

The bulk density of each ceramic membrane was calcu-

lated from its weight-to-volume ratio. The porosity was

measured using the Archimedes method. The open porosity

and pore size distribution of several selected samples were

measured by means of mercury porosimetry (AutoPore IV

9500, Micromeritics, Norcross, GA, USA). The microstruc-

tures of the samples were observed by scanning electron

microscopy (SEM, S4300, Hitachi Ltd., Hitachi, Japan). X-

ray diffraction (XRD, D8 Discover, Bruker AXS GmbH, Ger-

many) was conducted on the ground powders using CuKα

radiation. For flexural strength measurements, bar-shaped

samples were cut to a size of 4 mm × 5 mm × 30 mm. Bend-

ing tests were performed at a crosshead speed of 0.5 mm/min

using a three-point bending fixture with a span of 20 mm.

The permeability of several selected samples was mea-

sured by a capillary flow porometer (CFP-1100-AEX, PMI,

New York, USA), and the gas permeability (α, specific per-

meability) was computed from the measured flow rate and

pressure difference using Darcy’s law,

∆p/L = η·Q/A·α (1)

where ∆p is the pressure drop from the entrance to the exit

of the sample, L is the thickness of the sample, Q is the flow

rate of air through the sample, η is the viscosity of air, A is

the cross-sectional area of the sample, and a is the perme-

ability. Samples with dimensions of 3 × 30 × 25 mm were

fixed in a sample holder with an O-ring and adhesive. Based

on Eq. (1), the permeability was calculated from the slope of

the line of the plot of ∆p vs. Q.

3. Results and Discussion

The XRD analysis of the samples showed that the starting

clay powder was composed of kaolinite and sillimanite

phases (Fig. 1 (a)). There was no phase change during sin-

tering in the SB0 and SB5 samples, except for the SB5 sam-

ple, which was sintered at 1200oC (Fig. 1(b)). The XRD data

of this sample (Fig. 1 (b)) clearly show the formation of α-

cristobalite. This indicates that the addition of sodium

borate in an excess amount (5 wt% in this case) promotes

the formation of α-cristobalite, which may be derived from

the partial decomposition of the sillimanite and/or kaolinite

phases in the presence of molten sodium borate.

The effect of the sintering temperature on the microstruc-

ture of the clay-based membranes (SB3) is shown in Fig. 2.

The microstructures consisted of large kaolin grains and a

sodium borate bonding phase. The pressed compacts were

heat-treated at 900-1200oC for 2 hr in air at a heating rate

of 3oC/min. The heat treatment facilitated the melting of the

sodium borate, and the molten sodium borate acted as a glue to

bind the kaolin particles together. As shown in Fig. 2(d), kaolin

particles were well bonded to each other by the molten

sodium borate phase. The SB3 sample, sintered at 1200oC

and with a porosity of 25%, consisted of strongly intercon-

nected kaolin grains and large pores (Fig. 2(d)), whereas the

SB3 sample, sintered at 900oC and with a porosity of 44%,

consisted of loosely interconnected kaolin grains and small

pores (Fig. 2(a)). The fracture mode changed from inter-

granular to transgranular with an increase in the sintering

temperature from 900oC to 1200oC, indicating that the degree

of bonding between the kaolin particles became stronger with

an increase in the temperature. Sodium borate was trans-

formed into a viscous liquid phase during sintering with lit-

tle volume shrinkage and with the kaolin particles bound

Table 1. Batch Composition and Sample Designation

Sample Designation Composition (wt%)

SB0 100% kaolin†

SB1 99% kaolin + 1% sodium borate‡

SB2 98% kaolin + 2% sodium borate



†Samchun Pure Chemical Co. Ltd., Pyongtak, Korea ‡Shinyo Pure Chemical Co. Ltd., Hyogo, Japan

September 2013 Processing of Kaolin-Based Microfiltration Membranes 343

together.29) Moreover, it was clearly visible that the pore size

and pore structure changed with an increase in the sinter-

ing temperature. The structure of the kaolin-based mem-

branes became dense and the pore size of the membranes

increased with an increase in the sintering temperature.

Fig. 3 shows the pore size distribution of the SB3 samples

sintered at 1000oC, 1100oC, and 1200oC. This result shows a

unimodal pore size distribution for all samples. The average

pore diameter increased from 0.30 µm to 0.41 µm with an

increase in the sintering temperature from 1000oC to

1200oC. This type of pore growth during an increase in the

sintering temperature is frequently observed in many other

porous ceramics.21,30,31) The pore growth was attributed to

the pore coalescence occurring during the sintering process.

The average pore sizes, ranging from 0.30 to 0.41 µm, corre-

spond to the pore size of the ceramic membranes for micro-

filtration.

The effect of the sodium borate content on the microstruc-

Fig. 1. XRD patterns of kaolin-based membranes sintered atvarious temperatures with (a) 0 wt% and (b) 5 wt%sodium borate.

Fig. 2. Typical fracture surfaces of kaolin-based membranes(SB3) fabricated at various temperatures: (a) 900oC,(b) 1000oC, (c) 1100oC, and (d) 1200oC.

Fig. 3. Pore size distribution of kaolin-based membranes(SB3) sintered at (a) 1000oC, (b) 1100oC, and (c)1200oC.


ture of clay-based membranes is shown in Fig. 4. The micro-

structure of the SB0 sample, sintered at 1100oC, consisted

of loosely interconnected plate-shape kaolin grains, whereas

the microstructure of the SB5 specimen consisted of well-

interconnected plate-shaped kaolin grains. This was due to

the difference in the fracture behavior. Mostly intergranu-

lar fracture was observed in the SB0 sample (no sodium

borate added), whereas mostly transgranular fracture was

observed in the SB5 sample (5 wt% sodium borate added). A

greater amount of sodium borate added led to stronger

bonding between the kaolin grains, resulting in a higher

potential for the generation of transgranular fractures. The

strong bonding between the kaolin grains was due to the

formation of a vitreous mass by fused sodium borate and

some of the impurities present in the kaolin. The starting

kaolin powder contained impurities of 0.04% Cl, 0.05% Fe,

0.005% heavy metals, and 0.0002% As.

Fig. 5 shows the porosity of the kaolin-based membranes

as a function of the sintering temperature. The porosity of

the kaolin-based membranes ranged from 25% to 46%

depending on both the sintering temperature and the

sodium borate content. It was observed that the porosity

decreased slightly from 900 to 1100oC later decreasing rap-

idly from 1100 to 1200oC. The dramatic decrease from 1100

to 1200oC was due to the enhanced densification of the

kaolin-based membranes at 1200oC. The particles tend to

agglomerate, leading to a more consolidated ceramic body at

1200oC.20,21,32) The porosity range obtained at different sin-

tering temperatures decreased from 34-46% to 25-40% with

an increase in the additive content from 1 to 5 wt%. A

greater sodium borate addition promoted the densification

of the membranes and decreased the porosity. The lowest

porosity (25%) was obtained when the membrane contain-

ing 5 wt% sodium borate was sintered at 1200oC due to the

partial filling of the pores by the viscous sodium borate flow

and the resultant densification. A similar trend was also

observed in sodium borate-bonded SiC ceramics.29)

The flexural strength of the kaolin-based membranes at

different sintering temperatures is shown in Fig. 6. In gen-

eral, the flexural strength trend was opposite to that of the

porosity, ranging from 0.3 to 28.4 MPa. The strength gener-

ally increased with an increase in the sintering temperature

and the additive content. The increase in strength was

mainly due to the enhanced densification, i.e., decreased

porosity. However, the flexural strength of the SB5 samples

increased from 7.8 MPa to 19 MPa with an increase in the

sintering temperature from 900oC to 1100oC, decreasing to

11.6 MPa when sintered at 1200oC. When we observed the

surface of the SB5 sample sintered at 1200oC by means of

SEM, many cracks on the surface were observed (see Fig. 7).

These types of cracks were not observed in any of the other

samples. XRD data of the sample (Fig. 1 (b)) clearly showed

the formation of α-cristobalite. Thus, the cracks observed in

the specimen were attributed to the phase transformation of

the cristobalite as the sample cooled. Thus, an addition of

sodium borate to kaolin exceeding the optimum content

(most likely 3 wt% in the case) led to the formation of α-cris-

tobalite, resulting in a decrease of the flexural strength. The

Fig. 4. Typical fracture surfaces of kaolin-based membranes sin-tered at 1100oC with various additive contents: (a) 0 wt%,(b) 1 wt%, (c) 2 wt%, and (d) 5 wt%.

Fig. 5. Porosity of kaolin-based membranes sintered with 0-5 wt% sodium borate as a function of sintering tem-perature.

Fig. 6. Flexural strength of kaolin-based membranes sin-tered with 0-5 wt% sodium borate as a function ofsintering temperature.


highest flexural strength (28.4 MPa) was obtained in the

SB3 sample sintered at 1200oC. This strength is comparable

to the strength values obtained in membranes prepared

with Moroccan clay and kaolin-quartz mixtures.19,21) Flex-

ural strengths of 10 MPa at a porosity level of 42% and 12

MPa at a porosity level of 35% have been reported in clay-

based membranes.19) Ceramic membranes fabricated using

kaolin, quartz, and calcium carbonate showed flexural

strengths of 34 MPa at 30% porosity21) and 11 MPa at 39%

porosity.

33) Cordierite membranes showed flexural strengths of

7 MPa at 46% porosity and 30 MPa at a porosity level of

38%.32) The present results suggest that the addition of

sodium borate will increase the strength of kaolin-based

membranes when they are sintered at 900-1200oC in air.

Fig. 8 shows the specific air flow rate of the kaolin-based

membranes sintered at 1100oC for 2 h. The specific flow rates

of the SB0, SB3, and SB5 samples at a ∆p of 30 psi were

0.0025 L/min/cm2, 0.0020 L/min/cm2, and 0.0010 L/min/cm2,

respectively. The flow rate of the membranes decreased

with an increase in the additive content in the starting com-

position. The specific flow rate of the SB0 sample sintered at

1100oC(0.0025 L/min/cm2) was 2.5 times higher than that of

the SB5 sample sintered at 1100oC(0.0010 L/min/cm2). The

porosities of SB0 and SB5 samples were 43% and 37%,

respectively. The permeabilities of the clay-based mem-

branes are shown in Fig. 9. The permeabilities of the SB0, SB3,

and SB5 samples sintered at 1100oC were 2.64 × 10−17 m2,

1.85 × 10−17 m2, and 1.36 × 10−17 m2, respectively. From Eq. (1),

it is clear that the permeability is proportional to the flow

rate. Specific permeability data based on Darcy’s law has

not been reported yet for clay-based membranes. Permeabil-

ities ranging from 10−12 to 10−13 m2 were reported in macro-

porous SiC34) and mullite-bonded SiC ceramics with micron-

size pores.35) Compared to the permeability of porous SiC,

the permeabilities of the clay-based membranes are low. A

further improvement in the permeability should be achieved

by manipulating the porosity and pore size distribution.

This can be realized by selecting the additive composition

judiciously and by using clay powders with well-controlled

particle size distributions.

4. Conclusions

Kaolin-based membranes with a pore size of 0.30-0.40 µm

were successfully prepared by a simple pressing route using

low-cost starting materials, kaolin and sodium borate. The

present results suggest that ceramic membranes for micro-

filtration can be processed by a simple uniaxial pressing

method with low-cost raw materials. The flexural strength

increased with an increase in the sintering temperature and

the additive content, whereas the porosity decreased as the

sintering temperature and additive content increased. Both

the air flow rate and the permeability decreased with an

increase in the sodium borate content. The typical porosity,

flexural strength and specific flow rate of a kaolin-based

membrane sintered with 3 wt% sodium borate at 1200oC

were 25%, 28 MPa, and 2 × 10−3 L/min/cm2 at a ∆p of 30 psi,

respectively.

Fig. 7. Surface micrograph of kaolin-based membranes (SB5)fabricated at 1200oC. Note the occurrence of crackingon the surface of the sample.

Fig. 8. Specific flow rate of kaolin-based membranes sin-tered at 1100oC as a function of the pressure drop(∆p).

Fig. 9. Air permeability of kaolin-based membranes fabri-cated at 1100oC for 2 h in air.


Acknowledgment

This work was supported financially by the Fundamental

Research Program of the Korea Institute of Materials Sci-

ence (KIMS).

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