S E P A R A T I ON S : MA T E R I A L S , D E V I C E S A ND P RO C E S S E S

Simultaneously enhancing interfacial adhesion andpervaporation separation performance of PDMS/ceramiccomposite membrane via a facile substrate surface graftingapproach

Guining Chen | Haipeng Zhu | Yingting Hang | Quan Liu | Gongping Liu |

Wanqin Jin

State Key Laboratory of Materials-Oriented

Chemical Engineering, College of Chemical

Engineering, Nanjing Tech University, Nanjing,

China

Correspondence

Dr Gongping Liu, State Key Laboratory of

Materials-Oriented Chemical Engineering,

College of Chemical Engineering, Nanjing Tech

University, 5 Xinmofan Road, Nanjing 210009,

China.

Email: gpliu@njtech.edu.cn

Funding information

Topnotch Academic Programs Project of

Jiangsu Higher Education Institutions (TAPP);

Ministry of Education of China, Grant/Award

Number: IRT17R54; National Natural Science

Foundation of China, Grant/Award Numbers:

21490585, 21776125, 21922805; National

Key Basic Research Program, Grant/Award

Number: 2017YFB0602500

Abstract

A facile substrate surface silane-grafting approach was demonstrated to enhance both

interfacial adhesion and pervaporation separation performance of PDMS composite

membrane. With C16 grafted ceramic substrate, the PDMS/ceramic composite mem-

brane exhibited up to 1.7 times stronger interfacial adhesion force between separation

layer and substrate layer, meanwhile 1.5 times larger butanol/water separation factor

that is higher than state-of-the-art membranes. This novel approach paves a new ave-

nue to developing composite membranes with high and stable separation performance.

K E YWORD S

butanol recovery, ceramic hollow fiber, interfacial adhesion, PDMS membrane, surface

grafting

1 | INTRODUCTION

Separation is an essential process in chemical industry, among which

membrane technology can lower global energy use and reduce carbon

dioxide footprint.1 However, it remains challenge to develop high-

performance membranes enabling replacement of conventional sepa-

ration processes.2 Although a great number of membrane materials

with outstanding transport properties (permeability) have been devel-

oped, most of them for gas or vapor separation are based on symmet-

ric membrane with a thick separation layer, and thus providing a low

permeance (or flux) during realistic separation process.3 To realize a

high-efficiency separation process, a thin-film composite (TFC) mem-

brane is often required, consisting of a thin selective layer supported

on a porous substrate.

Two methods are often used to fabricate TFC membranes: Interfa-

cial polymerization and surface coating.4 Rubbery polymers, such as

polydimethylsiloxane (PDMS) and polyether block amide (PEBA), have

been widely used for pervaporation separation of volatile organic

compounds (VOCs)5 and gas separations (e.g., O2/N2, H2/CO2).3 They

are fabricated into TFC membranes mainly based on surface coating

approach, whose structural stability is of great concern due to the dif-

ferent swelling properties6,7 and/or interfacial incompatibility8

between selective layer and substrate. Thus, this kind of TFC mem-

branes is prone to be delaminated as applied in practical separation

process.6 A transition layer is usually introduced to enhance the inter-

facial adhesion of composite membranes by creation of ionic9 or

chemical bonding7,10 between selective layer and substrate. However,

preparation of the transition layer would complicate the membrane

fabrication process, and meanwhile, introduce additional transport

resistance causing loss of flux. Another general challenge forGuining Chen and Haipeng Zhu contributed equally to this study.

Received: 31 December 2018 Revised: 14 August 2019 Accepted: 24 August 2019

DOI: 10.1002/aic.16773

AIChE Journal. 2019;65:e16773. wileyonlinelibrary.com/journal/aic © 2019 American Institute of Chemical Engineers 1 of 6

https://doi.org/10.1002/aic.16773

developing high-performance TFC membranes is formation of a thin

and defect-free selective layer on a macroporous substrate.4 Dilute

polymer solution could reduce the membrane thickness to increase

the permeance. However, it may also inevitably suffer the polymer

penetrating into the substrate pores,11 which would result in defects

to lower the selectivity and higher transport resistance to sacrifice the

permeance.12 Recently, a sacrificial nanostrand layer was delicately

deposited on top of an ultrafiltration substrate to realize fabrication of

an ultrathin polyamide separation layer providing ultrafast molecular

transport.13 Nevertheless, removal process of the sacrificial

nanostrand layer might damage the separation layer and thus remains

challenging for most TFC membranes.

In this work, alternatively, we propose a facile substrate surface

grafting approach to simultaneously enhance interfacial adhesion and

separation performance of PDMS/ceramic composite membrane.

Specifically, it is realized by grafting long alkane chains (C16) onto the

surface of ceramic substrate to enhance the molecular interaction

between the surface groups of the substrate and PDMS chains of the

separation layer, and meanwhile create an organophilic surface

to improve the wetting and spreading of PDMS solution on the

substrate.

2 | SUBSTRATE SURFACE GRAFTING ANDCOMPOSITE MEMBRANE FORMATION

As shown in Figure 1a, a macro-porous Al2O3 hollow fiber (average

pore size � 1,100 nm)14 was modified with 5 wt% hexadecy-

ltrimethoxysilane (HDTMS)/ethanol solution for 4 hr and then annealed

at 120�C for 12 hr. The surface hydroxyl groups of Al2O3 substrate was

reacted with the methyoxyl groups of HDTMS to form Al O Si cova-

lent bond. HDTMS has been used to modify porous inorganic mem-

brane (TiO2, Al2O3) to create a hydrophobic surface for separation of

nonpolar organic solvents15 or membrane distillation.16 Alternatively,

the long C16 chains attached on the substrate surface aim to interact

with PDMS chains to provide considerable interfacial interactions for

the final PDMS/ceramic composite membrane. From the IR analysis

(Figure S1), it is found that after modification the ceramic substrate

shows new peaks at 2,944 and 2,876 cm−1 corresponding to the C H

stretching vibrations from CH3 and CH2 , and 910 cm−1

corresponding to the characteristic peak of Si O C (Figure S1b). This

result combined with the spectrum of HDTMS (Figure S1c) indicate

successful grafting of the alkane chains on the ceramic substrate. The

formation of Al O Si bond was further confirmed by XPS characteri-

zation. In the Al 2p scan, there is a new peak at 76.48 eV corresponding

to the Al O Si bonding17 in HDTMS modified ceramic substrate

(Figure S2). Furthermore, in the O 1s scan, new peaks appear at 531.13,

531.95, and 533.68 eV, which are related to Si O C, Si OH, and

Si O Si bonds, respectively18,19 (Figure S3). It suggests that there are

some unreacted methyoxyl groups, hydrolytic methyoxyl groups, and

reaction between two methyoxyl groups to form Si O Si bond.

The long alkane chains on the surface could regulate surface prop-

erty of the ceramic substrate, which is evidenced by the contact angle

test. Water was dropped on the substrate surface to measure the

hydrophobicity. As shown in Figure 1b, the water contact angle on

the unmodified substrate becomes 0� within 1 s, suggesting a very

hydrophilic surface due to the surface hydroxyl groups (Al–OH). After

HDTMS grafting, the ceramic substrate surface is transformed to be

very hydrophobic, showing a stable water contact angle of 145�,

which is resulted from super-hydrophobicity of the surface attached

F IGURE 1 Design and fabrication of PDMS membrane supported on surface-grafted ceramic substrate: (a) ceramic hollow fiber substrate issurface grafted with C16 chains using hexadecyltrimethoxysilane (HDTMS) and then dip-coated with PDMS solution to form PDMS/ceramichollow fiber composite membrane; (b) water contact angle on the surface of unmodified and modified ceramic substrate; (c) typical SEM imagesof cross-section of PDMS selective layer supported on the modified ceramic hollow fiber substrate [Color figure can be viewed atwileyonlinelibrary.com]

2 of 6 CHEN ET AL.

C16 chains rather than the changes of surface nanostructure

(Figure S4). These C16 chains meanwhile make the substrate surface

very organophilic that exhibit high affinity towards PDMS solution

using n-heptane as the solvent, as confirmed by the low contact angle

of n-heptane on the modified ceramic substrate (19.8� shown in

Figure S5). Thus, the wetting and spreading of PDMS solution on the

surface of ceramic substrate could be significantly improved during

the coating process of composite membrane preparation. Therefore, a

homogenous PDMS separation layer was easily deposited on the sur-

face of ceramic hollow fiber substrate via a facile dip-coating method.

As displayed in Figure 1c, a uniform hollow fiber structure is observed

for the PDMS/ceramic composite membrane. The ceramic hollow

fiber substrate has an asymmetric porous structure consisting of

sponge-like pores on the top and finger-like pores underneath

(Figure S6), which offer smooth coating surface and low transport

resistance, respectively.9 Typically shown in Figure 1c, an even PDMS

separation layer with controlled thickness is coated on the outer

surface of the porous ceramic substrate.

3 | INTERFACIAL ADHESION OFCOMPOSITE MEMBRANES

To probe interfacial adhesion of the as-prepared PDMS/ceramic

composite membrane, we first employed molecular dynamics

(MD) simulation to study the interfacial molecular interaction of

PDMS chains with ceramic (Al2O3) surface before and after surface

grafting of C16 chains.20 The constructed PDMS–unmodified ceramic

interface and PDMS–C16 modified ceramic interface models are given

in Figure 2a,b, respectively. According to the thermodynamics theory,

the interaction energy ΔE can be calculated as: ΔE = EPDMS-substrate

– (EPDMS + Esubstrate), where EPDMS-substrate is the energy of PDMS-

substrate interface; EPDMS and Esubstrate are the energies of the

equilibrated PDMS and substrate, respectively. The calculation results

in Table 1 indicate that the interaction energy between the PDMS

and substrate is enhanced by 14 times after grafting C16 on the sub-

strate surface, from −318.8 to −5,652.5 kcal/mol. Both the van der

Waals and electrostatic interactions are improved in the PDMS-

modified substrate interface, where the electrostatic interaction based

on locally charged atoms (Scheme S2a)21 dominates the enhancement

of interfacial interaction.

With the above atomic-level understanding, we then experimentally

probed the interfacial adhesion behavior of the composite membranes

using an in situ nanoindentation/scratch technique22 (Figure 2c). The

measurement monitors and records the scratch distance relationships

with the dynamic load, friction force, and corresponding friction coeffi-

cient. As shown in Figure S7, critical load at the failure is considered as

the interfacial adhesion force of the PDMS layer onto the ceramic sub-

strate. More details of the nanoindentation/scratch measurements are

provided in the Supporting Information. Figures 2d,e presents typical

scratch morphologies of the PDMS/ceramic composite membranes by

ramping the critical load to maximum. It can be directly seen that the

cracking of the PDMS-substrate interface is significantly reduced in the

surface modified substrate supported PDMS composite membrane. To

quantify the interfacial strength, we further measured the critical loads

of PDMS/ceramic composite membranes with membrane thickness

F IGURE 2 Interfacial adhesion between PDMS layer and ceramic substrate: (a) unmodified and (b) surface modified ceramic-PDMS interfacemodels constructed by molecular dynamics simulation (“in-cell” display style) to calculate the interfacial interaction energy; (c) schematic ofnanoindentation/scratch test on the PDMS/ceramic composite membrane to measure the interfacial adhesion force; SEM images of surfacescratch morphology of PDMS membrane layer supported on (d) unmodified and (e) surface modified ceramic hollow fiber substrate; (f) measuredinterfacial adhesion force of PDMS membranes with various thicknesses supported on unmodified and surface modified ceramic hollow fibersubstrate. The values for unmodified samples are adopted from our previous study22 [Color figure can be viewed at wileyonlinelibrary.com]

CHEN ET AL. 3 of 6

from 5 ± 0.2 to 12 ± 0.3 μm prepared by varying coating viscosity from

3.0 to 15 cP (Figure 2f). Generally, the composite membrane with

thicker PDMS layer exhibits higher interfacial adhesion, which is consis-

tent with our previous study.22 Film thickness is a key parameter

influencing the critical load (interfacial adhesion) in the nanoscratch test.

In principle, film thickness can have two opposing effects: Thicker films

that are harder than the underlying substrate provide more load support

and so delay the onset of the substrate deformation that is often the

precursor of film failure (higher critical load); and thicker films can be

more highly stressed and more easily through thickness crack and

delaminate when deformed (lower critical load) since the driving force

for spallation to reduce stored elastic energy is greater.

Notably, with the same thickness (e.g., 5 ± 0.2 μm), PDMS layer

coated on the surface-modified ceramic hollow fiber achieves stron-

ger interfacial adhesion than that on the unmodified substrate

(e.g., 30.67 mN vs. 17.9 mN). The enhancement is more remarkable

for the composite membrane with thinner PDMS layer, which is par-

ticularly favorable for developing composite membrane with thinner

membrane thickness and thus higher permeate flux. Noting that the

membrane thickness is thicker than recently reported PDMS thin-

composite membranes applied for flue gas and air separations,23

propane/propene separation24 and water vapor removal from air,25

which might be due to the diverse applications have different require-

ments in membrane thickness, as well as using different substrates to

fabricate the PDMS membrane.

Two possible reasons can be attributed to the enhanced interfacial

adhesion: (a) substrate surface grafted C16 chains interact with PDMS

chains20; (b) PDMS chains penetrating the substrate pores provide

mechanical interlocking.26 The first contribution has been verified by

the highly increased interfacial interaction energy of the composite

membrane using C16 grafted substrate according to the MD simula-

tion calculation (Figure 2a,b, Table 1). The second factor was studied

by comparing the penetration of PDMS into the porous substrate

before and after surface grafting C16. As shown in Figures S8 and S9,

there is little difference in the EDX line scans of Si element (only from

PDMS layer) for the cross-section of composite membrane supported

on unmodified and modified ceramic hollow fiber substrate,

suggesting a similar penetration of PDMS for both composite

membranes. Therefore, the significant improvement of interfacial

adhesion force probed in the PDMS membrane coated on the modi-

fied substrate is mainly owing to the highly enhanced molecular inter-

action between PDMS chains and ceramic substrate surface grafted

with C16 chains. It is noted that the measured interfacial adhesion

force between PDMS separation layer and ceramic hollow fiber sub-

strate is an actual parameter for determining the structural stability of

the resulting composite membrane, whereas the calculated interaction

energy between PDMS and (unmodified or modified) ceramic is used

to understand the interfacial interaction mechanism.

4 | SEPARATION PERFORMANCE OFCOMPOSITE MEMBRANES

The separation performance of PDMS/ceramic composite membranes

was evaluated by pervaporation recovery of butanol from aqueous

solution—A key process for in situ concentrating butanol from bio-

mass fermentation process of biobutanol production.27 Typical sepa-

ration conditions (i.e., operating temperature and feed composition)

were chosen to simulate the biobutanol recovery process from its fer-

mentation broth. As shown in Figure 3a, increasing the membrane

thickness generally reduces the total flux while increases the separa-

tion factor [YA/YB/(XA/XB), Yi and Xi are the weight fractions of

components in permeate and feed side, respectively; A: n-butanol; B:

water]. The thickness-dependent flux is reasonable according to the

Fick's law that membrane flux is in inverse proportion to its thickness.

While the higher separation factor with thicker membrane indicates

that some minor defects were eliminated as increasing the separation

layer thickness. These defects might be produced by the nonideal

coating of PDMS solution on the surface of substrate. As discussed

above, the wetting and spreading of PDMS solution can be highly

improved by regulating the surface wettability with the aid of grafting

organophilic C16 chains on the substrate. As expected, the separation

factor of the PDMS composite membranes coated on modified sub-

strate is much higher than using the unmodified substrate. For

instance, the separation factor for �12 ± 0.3 μm-thick PDMS compos-

ite membrane is improved from 36 to 53 by using the surface C16

grafted substrate. The slightly lower total flux in the modified hollow

fiber supported PDMS composite membrane is actually due to the

desirable suppression of water flux compared with the unmodified

hollow fiber supported membrane, as shown in Figure 3b.

Compared with reported membranes for butanol recovery, our

ceramic hollow fiber supported PDMS composite membranes exhibit

good separation performance (blue dash line in Figure 3c), especially

high flux, owing to the thin PDMS layer and low transport resistance

of the ceramic hollow fiber. Notably, the substrate surface grafting

approach preserves the high flux while further enhances the separation

factor of PDMS/ceramic hollow fiber composite membrane (red solid

line in Figure 3c). To show the great potential in practical application,

we further applied the surface modified ceramic hollow fiber supported

PDMS composite membrane with enhanced interfacial adhesion and

separation performance for recovering acetone–butanol–ethanol (ABE)

TABLE 1 Interaction energies between PDMS and substrate

ModelTotal energy(kcal/mol)

van der Waals(kcal/mol)

Electrostatic(kcal/mol)

PDMS −2,655.9 −206.1 −3,096.5

Unmodified substrate −43,746.3 −35,620.2 −8,178.3

C16 modified substrate −41,737.0 −33,778.8 −8,186.2

PDMS-unmodified

substrate

−46,783.9 −39,871.2 −11,290.5

PDMS-modified

substrate

−50,045.4 −39,465.6 −11,571.6

EPDMS-unmodified substrate −381.8 −4,044.9 −15.8

EPDMS-modified substrate −5,652.5 −5,480.7 −288.9

4 of 6 CHEN ET AL.

solvents that are full products in biobutanol fermentation process.

As expected, the membrane performance is excellent and stable

during more than 100 hr continuous operation, with a total flux

�1,081 g/m2 hr and separation factor [YA/YB/(XA/XB), Yi and Xi are

the weight fractions of components in permeate and feed side,

respectively; A: acetone, n-butanol or ethanol; B: water] for acetone

�28.1, for butanol �28.9, and for ethanol �6.2 (Figure 3d). Neverthe-

less, longer operation time would be required to obtain a more compre-

hensive structural stability during separation process.

5 | CONCLUSIONS

In summary, we have demonstrated a facile substrate surface grafting

approach simultaneously enhancing interfacial adhesion and separation

performance of PDMS/ceramic composite membrane. The long orga-

nophilic alkane chains (C16) grafted on the substrate surface highly

enhanced the molecular interaction and thus interfacial adhesion (up to

1.7-fold) between substrate with PDMS separation layer; meanwhile

significantly improved the wetting and spreading of PDMS solution on

the substrate to afford much larger butanol/water separation factor

(up to 1.5-fold) without loss of flux in the PDMS/ceramic hollow fiber

composite membrane that is higher than state-of-the-art polymeric

membranes. This novel approach might open a new door to developing

highly permeable, selective, and stable composite membranes.

ACKNOWLEDGMENTS

This work was financially supported by National Key Basic Research

Program (2017YFB0602500), National Natural Science Foundation of

China (Nos. 21922805, 21776125, 21490585), Innovative Research

Team Program by the Ministry of Education of China (No. IRT17R54)

and Topnotch Academic Programs Project of Jiangsu Higher

Education Institutions (TAPP).

ORCID

Gongping Liu https://orcid.org/0000-0002-3859-1278

Wanqin Jin https://orcid.org/0000-0001-8103-4883

F IGURE 3 Separation performance of PDMS/ceramic hollow fiber composite membrane: Effect of substrate surface grafting and membranethickness on (a) the total flux and separation factor and (b) individual flux for pervaporation separation of 1 wt% butanol/water mixtures at 40�C;(c) performance comparison with state-of-the-art polymeric membranes in literature for butanol recovery from aqueous solution, more details arelisted in Table S1; (d) a typical result of PDMS membrane supported on surface-modified substrate for continuous pervaporation separation ofacetone/butanol/ethanol/water (0.6/1.2/0.3/98 wt%) mixtures at 40�C. The values for unmodified samples are adopted from our previousstudy22 [Color figure can be viewed at wileyonlinelibrary.com]

CHEN ET AL. 5 of 6

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SUPPORTING INFORMATION

Additional supporting information may be found online in the

Supporting Information section at the end of this article.

How to cite this article: Chen G, Zhu H, Hang Y, Liu Q, Liu G,

Jin W. Simultaneously enhancing interfacial adhesion and

pervaporation separation performance of PDMS/ceramic

composite membrane via a facile substrate surface grafting

approach. AIChE J. 2019;65:e16773. https://doi.org/10.1002/

aic.16773

6 of 6 CHEN ET AL.