The surface modification of polyamide membranes using graphene oxide

Journal Pre-proof The surface modification of polyamide membranes using graphene oxide Anna Kowalik-Klimczak, Ewa Woskowicz, Joanna ´ Kacprzynska-Gołacka

PII:

S0927-7757(19)31276-2

DOI:

https://doi.org/10.1016/j.colsurfa.2019.124281

Reference:

COLSUA 124281

To appear in:

Colloids and Surfaces A: Physicochemical and Engineering Aspects

Received Date:

7 October 2019

Revised Date:

22 November 2019

Accepted Date:

25 November 2019

´ Please cite this article as: Kowalik-Klimczak A, Woskowicz E, Kacprzynska-Gołacka J, The surface modification of polyamide membranes using graphene oxide, Colloids and Surfaces A: Physicochemical and Engineering Aspects (2019), doi: https://doi.org/10.1016/j.colsurfa.2019.124281

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The

surface

modification

of

polyamide

membranes

using graphene oxide

Anna Kowalik-Klimczak*, Ewa Woskowicz, Joanna Kacprzyńska-Gołacka

ŁUKASIEWICZ Network Research - Institute for Sustainable Technologies, Poland

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*Corresponding authors: [email protected]

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Graphical Abstract

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HIGHLIGHTS  The surface of polyamide membranes were modified with graphene oxide (GO). The plasma activation in Ar-O2 mixture allowed GO to be attached to the membranes surface.



The membranes after treatment revealed antibacterial properties and high water permeability.

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

ABSTRACT

This paper presents the results of the surface modification of polyamide membranes using graphene oxide (GO) for reducing bacterial contamination. Prior to GO deposition on the surface of the membrane plasma treatment was used with a mixture of argon and oxygen (ArO2) to activate the surface of the flat sheet membranes. As a result, the process conditions for plasma activation were selected, which allow GO to be attached to the surface of polyamide

membranes. In the study, the effect of a deposition of GO aqueous dispersion on filtration, antibacterial properties and morphology of produced materials was investigated. The elaborated conditions allowed to obtain membranes with antibacterial properties and high water permeability.

Keywords: polyamide membranes, plasma activation, graphene oxide, antibacterial properties INTRODUCTION

Polymer membranes are used to separate particles of both liquid and gas mixtures ranging

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from single ions to tens of micrometers. They are composed of specific compartments separating individual components of the separated solutions and have been widely used in many sectors, including food, chemical, pharmaceutical, as well as medicine and biotechnology [1,2]. Pressure driven membrane processes are considered one of the best

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existing solutions to prevent water scarcity [1-3]. Therefore a lot effort is made to recover water from industrial wastewater and recycling, preferably in a closed loop [4-6] or seawater

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desalination to produce of drink water [7,8]. However, the key problem of the widespread use of membrane techniques in a large-scale plants is the cost of recovery of water to be reused.

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During the process of water recovery in membrane systems, a decrease in a permeate flux may occur in time due to the deposition of filtered liquid components on the membrane surface or in its internal structure [9-16]. This phenomenon results in a reduction of filtration

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efficiency, chemical cleaning of contaminated membrane and, finally replacement of a membrane. Due to the high intensity contamination during operation and related problems with cleaning, lifetime of a membrane is significantly shortened. In addition, due to the

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decrease in efficiency, it is necessary to use either a larger membrane surface or higher transmembrane pressure, which results in greater energy consumption and increased

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investment and operating costs. In order to solve these problems the modifications can be introduced to the surface of the membrane, which might reduce significantly deposited pollutants on the membrane surface. According to the literature data [16-20] and conducted research [21-23], it is possible to modify the surface of polymer membranes physically using gas or metallic plasma, chemically using appropriate solutions or using a combination of both. Plasma modification involves the treatment of the polymer surface with a variety of ionized gases, i.e. CO 2, Ar, CF4, Ar-CH4, CH4-N2 [24-26] or the application of discrete layers of coatings such as silver

(Ag) [17], titanium (Ti) [22], copper oxide (CuO) [23,27]. Plasma treatment is also commonly used to activate the polymer surface functional groups prior to chemical modification via grafting reaction of hydrophilic macromolecules, e.g. polyethyleneimine, polyacrylic acid or polyethylene oxide [28]. This type of surface modification of polymer membranes leads to the appearance of functional groups whose charge depends on the pH of the solution. Nanostructures with antibacterial and photocatalytic properties, i.e. titanium dioxide (TiO2), zinc oxide (ZnO), silver oxide (AgO) have also been used to modify the surface of polymer membranes [4,18,29,30]. In recent years, the production of graphene form-containing polymeric membranes increased,

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[31-37]. Possibilities of using graphene or graphene oxide (GO) to manufacture and modify membranes are primarily due to the fact that it is impermeable to most substances except water. In addition, graphene's unique property is the mechanical strength and reactivity, which enables to create composite materials. Graphene primarily in oxidized form also shows antimicrobial properties [37-39]. This is extremely important property as membranes used for

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water and wastewater treatment are often exposed to biofouling resulting from microbial growth. Along with the availability of appropriate nutrients in feed water, microorganisms can

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freely multiply on the surface of the membrane leading to deterioration of filtration properties.

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The purpose of the work was to elaborate specific conditions of surface modification of polymer membranes using GO to impart antimicrobial properties. Prior to modification with GO the conditions of plasma were selected to treat the surface of polymer membranes with

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mixture of gases (Ar-O2).

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EXPERIMENTAL

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The activation and modification techniques

The surface modification of membranes was obtained after two different processes. The first was activated using low-temperature non-metallic plasma obtained by low-pressure glow discharge technique. Plasma activation processes were carried out at the chamber, which was discussed in the work [23]. As part of the experimental work, a series of surface activation processes in non-metallic plasma was carried out using a working atmosphere consisting of a mixture of argon (90%) and oxygen (10%). The activation time of membranes in non-metallic

plasma was changed in the range of 30-150 s for process carried out pressure equal to 1 mbar. In the next stage, the pressure during plasma activation was changed in the range of 1-3 mbar for process carried out time equal to 120 seconds. The second process consisted of graphene oxide (GO) deposition on the surfaces of plasma-activated membranes using dip coating method, which is most commonly used in the industrial production of composite membranes for water and wastewater treatment. For surface modification of flat sheet polyamide membranes (MAGNA from GVS Filter Technology with 0.22 μm pore diameter), an aqueous dispersion of GO in the concentration of 0.5-4.0 g/dm3 was used, in which GO flakes are characterized by sizes of 5-30 μm

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(Nanopoz). Membranes after plasma activation and surface modification were compared to the reference materials (native membranes). The parameters, which were tested in the work were microstructure and chemical composition of the membrane surface, permeate flux and

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wettability to polar liquid as well as antibacterial properties.

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Membrane surface characterization

The microstructure of the membrane surface was characterized based on images recorded

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with two scanning electron microscopes: Hitachi TM 3000 TM table-top series equipped with BSE and Hitachi electron back-scatter detector with field emission with SU-70 Schottky. Before microscopic analysis, the surface of the non-conductive samples was coated with a

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layer of carbon about 20 nm thick (SCD 050 Sputter Coater, BAL-TEC). For qualitative analysis of membranes modified with GO aqueous dispersion, a Fourier Transform Infrared Spetrophotometer (FT-IR) from Perkin Elmer was used. The IR spectra

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was recorder (by reflection method) from a selected area of the surface. As the tests were performed in the air atmosphere, the spectra contained bands characteristic for carbon dioxide

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absorption (2430-2225 cm-1). Therefore, the obtained spectra were subjected to mathematical processing, using the Grams computer program, which removed these interfering signals, smoothing the spectrum by the Savitsky-Golay method and multipoint normalization of the baseline [40]. The surface composition of treated membranes and the chemical states of the contained elements [41-43] were performed using the X-ray Photoelectron Spectroscopy/Electron Spectroscopy for Chemical Analysis (XPS/ESCA) from Prevac, equipped with the VG Scienta R3000 hemispherical electron energy analyzer. Data acquisition was carried out in

SWEPT mode, with 200 eV transition energy and 200 meV for overview spectra and 50 meV for detailed spectra. XPS spectra reflect the number of electron counts (vertical) with a specific energy (horizontal) obtained from the surface of the tested sample. An achromatic Xray source was used with a double aluminum/magnesium anode operating at 200 W (8.4 kV, 24.0 mA). During the analysis, an aluminum anode was used, emitting radiation of the Kα1,2 line with the energy of 1486.6 eV. The analyzes were carried out under ultra-high vacuum conditions at a pressure not exceeding 3·10-12 bar. The relative quantitative share of individual elements in the surface layer was determined based on the analysis of the intensity of the main peaks. After recording the review electron spectrograms, the detailed spectrograms were

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recorded in the range of selected energy corresponding to the energy of electrons emitted by the elements typical for the sample. Calibration of the binding energy scale was based on the location of the C 1s carbon line corresponding to C-C and C-H bonds and was assumed to be 284.8 eV. In order to identify the chemical state of the detected elements, the detailed spectrograms were deconvoluted using Casa XPS software (line shape: Gaussian –

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Lorentzian, background type: Shirley) [44].

Filtration performance

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Permeate flux was determined by measuring the time needed to filter liquid (100 cm3) through the active membrane surface (8 cm2) under transmembrane pressure (500 mbar). For this

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purpose, ‘dead end’ filtration set-up was used. In contrast, the wettability of membranes with polar solvent was determined by measuring contact angle using the drop method (droplet volume 2 µL) using a tensiometer by ŁUKASIEWICZ Network Research - Institute for

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Sustainable Technologies (ŁUKASIEWICZ-ITEE). In the testing of membranes before and after modification, demineralized water was used, which had a specific conductivity and pH

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of 5.3 µS/cm and 6.5, respectively.

Microbiological experiments

Representative model microorganisms of Gram-negative bacteria Escherichia coli (ATCC 25922) were cultured in a flask containing 20 cm3 of Luria-Bertani (LB) broth at 37ºC in shaking incubator (Innova) for 24 h. The following day, the suspensions of bacteria were diluted with PBS to reach concentration of approximately 100 CFU/cm3. Prior to further

microbiological tests, the modified and reference membranes were sterilized for 30 minutes with a UV-C lamp in a laminar cabinet. Then, the bacterial suspension in the volume of 10 cm3 was filtered through membranes in the vaccum filtration set-up. After filtration, they were placed on Luria-Bertani (LB) agar plates and left in an incubator at 37°C for 24 h. Bacterial colonies grown on the membranes were counted as colony forming units (CFU) and the viability of bacteria on the membranes was determined with the following formula:

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The pieces of membranes were selected to observe the influence of GO on bacterial cells structure within bacterial colonies under scanning electron microscope (SEM). The chosen samples were prepared with the appropriate protocol for biological samples in order to maintain original structure of bacteria. The procedure was divided into three steps: fixation,

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dehydratation and critical point drying. For fixation, the samples were soaked in 3% glutaraldehyde in PBS (pH ≈ 7 at 4ºC for 16 h), 1% osmium tetroxide (OsO4 at 4ºC for 16 h)

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and demineralized water (3 series before and after OsO4 for 10 minutes each). In turn, for dehydratation, the samples were soaked in ethanol series (30%, 50%, 70%, 80%, 90%, 96%,

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100% for 10 minutes each) and acetone series (30%, 50%, 100% for 10 minutes each). Next, the samples were placed in porous containers bathed in ethanol and transferred into an automated critical point dryer (Leica EM CPD300) using CO2. CPD was performed with the

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program proposed by producer to bacteria [45]. Once finished, the samples of membranes were coated with 20 nm layer of gold. The analysis of the cell structure of bacteria was

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conducted using SEM (Hitachi TM 3000).

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RESULTS AND DISCUSSION

Plasma activation of polymer membranes

In the first step of the work, the effect of Ar-O2 activation time at 1 mbar was examined on the permeate flux of demineralized water (Fig. 1).

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Native membrane

Permeate flux, dm 3 /(m 2 s)

1.2

1.0

0.8

0.6

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0.4

0.2

0.0 30

60

90

120

150

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Time of plasma activation in Ar-O2 , s

Fig. 1. The influence of plasma activation time in Ar-O2 mixture on the permeate flux obtained for

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tested membranes during filtration of demineralized water.

Compared to the native membrane the permeate flux until 90 s of activation was higher, however the extension of activation time resulted in decrease of permeate flux (Fig. 1). It was

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caused by loosening of the membrane structure under the influence of applied process conditions (Fig. 2 a and b). After plasma activation for 120 s, the permeate flux was similar to that obtained during filtration of demineralized water through the native membrane (Fig. 1).

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This membrane was characterized by a structure similar to that observed for the native membrane (Fig. 2 a and c). However, the permeate flux obtained during the filtration of

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demineralized water through the membrane activated for 150 s was 17% lower than the permeate flux determined for the native membrane (Fig. 1). This was due to the condensing of the membrane structure, which was influenced by plasma process conditions (Fig. 2 a and d).

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Fig. 2. Surface structure of the native membrane (a) and membranes after plasma activation with Ar-

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O2 mixture conducted for 30 s (b), 120 s (c) and 150 s (d).

The changes observed in polymer structure (Fig. 2) most likely resulted from the formation of oxygen bridges and more uniform non-porous film on the polyamide surface. Due to the

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incorporation of oxygen into the structure, the volume of the polymer material increases leading to smaller ability to firmly attach GO to the membrane surface.

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In the next stage of the work, the influence of the pressure of the activation process of the polyamide membrane was examined on the permeate flux of demineralized water (Fig. 3), which was higher when applying higher pressure of the plasma surface activation. Plasma activation with an Ar-O2 mixture carried out at a pressure of 1 mbar caused a 5% increase in the permeate flux relatively to the native membrane. In turn, plasma carried out at 2 mbar and 3 mbar pressures resulted in the increase permeate flux by 17% and 18%, respectively (Fig. 3). This was due to loosening of the membrane structure as a result of plasma treatment with Ar-O2 mixture (Fig. 4).

1.4

Native membrane

1.0

0.8

0.6

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Permeate flux, dm 3 /(m 2 s)

1.2

0.4

0.0

1

2

3

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Pressure of plasma activation in Ar-O2 , mbar

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0.2

Fig. 3. The effect of pressure applied during plasma activation in Ar-O2 on the permeate flux obtained

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during filtration of demineralized water.

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(d)

Fig. 4. Surface structure of native membrane (a) and membranes activated in Ar-O2 plasma for 120 s at

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1 mbar (b), 2 mbar (c) and 3 mbar (d).

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Surface modification of polymer membranes

After initial plasma activation of the membranes in the Ar-O2 mixture, the effect of the concentration of the GO aqueous dispersion (0.5-4.0 g/dm3) deposited on the membranes was

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investigated on the filtration properties of the membranes determined for demineralized water. As a result of the experiments, the permeate flux decreased along with the increase in the

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concentration of GO aqueous dispersion (Fig. 5).This was due to the higher values of contact angles, which determines lesser wettability of the materials (Fig. 6). SEM observations have shown that GO embedded on plasma-activated membranes tends to form spatial networks.

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Furthermore, a significant effect of the concentration of aqueous GO dispersion on the surface structure of the membrane was observed (Fig. 7).

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The most favorable results were obtained when modifying membranes using a 0.5 g/dm3 GO aqueous dispersion after prior activation of their surface with an Ar-O2 mixture maintained at 1 mbar pressure for 120 s. This is due to the fact that the plasma activation parameters used

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did not change the structure of the polyamide membrane, but contributed to the GO binding on the membrane surface in an amount that did not reduce its filtration properties. Membranes modified in this way had similar filtration properties compared to native membrane (Fig. 5) and contact angle lower than 5° (Fig. 6), which is typical for superhydrophilic materials [46,47].

1.2

Native membrane

0.8

0.6

0.4

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Permeate flux, dm 3 /(m 2 s)

1.0

0.2

0.0 0.5

1.0

2.0

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Concentration of GO dispersion,

4.0 g/dm 3

Fig. 5. The influence of the concentration of GO aqueous dispersion used for the surface modification

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of the membrane on the permeate flux for filtration of demineralized water.

50

45

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40

25 20

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30

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Contact angel, º

35

15 10 5 0

0.5

1.0

2.0

Concentration of GO dispersion,

4.0 g/dm 3

Fig. 6. The impact of the concentration of GO aqueous dispersion on the wettability of the generated membranes.

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(d)

Fig. 7. Surface structure of the native membrane (a) and membranes modified with GO aqueous dispersion at a concentrations of 0.5 g/dm3 (b); 1.0 g/dm3 (c); 2.0 g/dm3 (d) and 4.0 g/dm3 (e).

The composition of the surface of membranes modified using GO dispersion

In testing GO-modified membranes using FT-IR the functional groups of hydroxyl (-OH), carbonyl (=C=O) and carboxyl (-COOH) were identified characteristic for the obtained filtration materials (Fig. 8). The intensity of the peaks for particular functional groups was dependent on the concentration of the GO aqueous dispersion used for surface modification of

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polyamide membranes.

Fig. 8. FT-IR spectra of surface modified membranes with a GO aqueous dispersion: 0.5 g/dm3 (a); 1.0

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g/dm3 (b); 2.0 g/dm3 (c) and 4.0 g/dm3 (d) after prior plasma activation in an Ar-O2 mixture.

XPS/ESCA analysis of GO modified membranes determined chemical composition of the obtained filtration materials. Review spectra of membrane surfaces modified with GO aqueous dispersion in concentrations: 0.5 g/dm3; 1.0 g/dm3; 2.0 g/dm3 and 4.0 g/dm3 were presented in Fig. 9. This allowed to conclude that the surface layers of the tested membranes were composed of carbon (C 1s), oxygen (O 1s) and nitrogen (N 1s). In turn, quantitative

analysis (Table 1) indicated that as the concentration of GO aqueous dispersion used for surface modification of the membrane increases, the proportion of oxygen (O 1s) increases,

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and the share of carbon (C 1s) and nitrogen (N 1s) decreases.

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Fig. 9. Overview spectra of surface polyamide membranes modified with GO aqueous dispersion at a

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concentration of 0.5 g/dm3 (a); 1.0 g/dm3 (b); 2.0 g/dm3 (c) and 4.0 g/dm3 (d).

Table 1. Relative content of atoms of elements on the surface of membranes activated in plasma and -

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modified with GO aqueous dispersion - based on quantitative analysis of XPS spectra Characteristic

Concentration of GO aqueous dispersion, g/dm3

peak

0.5

1.0

2.0

4.0

C 1s

74.97

17.29

16.42

16.39

O 1s

19.21

75.90

80.08

82.86

N 1s

5.12

6.81

3.50

0.75

Chemical bonds were analyzed with detailed XPS/ESCA spectra of individual elements recorded with high resolution. Detailed spectra of carbon appeared in surface-modified membranes using GO dispersion at 0.5 g/dm3; 1.0 g/dm3; 2.0 g/dm3 and 4.0 g/dm3 were shown in Fig. 10, respectively. Deconvolution of the C 1s peak for surface-modified membranes using GO dispersion in following concentrations: 1.0 g/dm3; 2.0 g/dm3 and 4.0 g/dm3 (Fig. 10) showed the presence of carbon in two chemical states: bands with 284.7 eV energy characteristic for C-C/C-H bonds. In contrast, 287.2 eV and 287.6 eV bands are typical for carbon-oxygen bonds (C=O). The results of the analysis of this peak are consistent with the results of the analysis of the peak derived from oxygen atoms. The analysis also

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revealed -NH moieties specific for the polyamide membrane.

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(d)

Fig. 10. Detailed spectra of polyamide membranes modified with GO aqueous dispersion at concentrations of 0.5 g/dm3 (a); 1.0 g/dm3 (b); 2.0 g/dm3 (c) and 4.0 g/dm3 (d).

Antibacterial properties of membranes modified with GO

Microbiological activity of tested materials was performed for representative microorganisms belonging to the group of Gram-negative bacteria (Escherichia coli). It was found that Escherichia coli showed a linear correlation between the survival of these bacteria and the concentration of the GO aqueous dispersion used for surface modification of membranes (Fig. 11) and only 10% reduction was observed for the membrane surface modified with 0.5 g/dm3 aqueous GO dispersion (Fig. 11). Thus, scanning electron microscope was used to test the influence of membranes modified with GO on the morphology of bacterial cells grown on the filter. In the case of membranes modified with 0.5 g/dm3 GO dispersion, Escherichia coli was found to only appear in the spaces between GO flakes (Fig. 12 c). It can

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be associated with the repulsive interactions between bacteria and GO coated samples, where the blockage of gas/ion exchange of bacteria entrapped between GO flakes appears [48,49]. However, as few as single colonies of Escherichia coli with a significantly altered cell membrane structure were observed on GO flakes deposited on the membrane (Fig. 12 d and e). As a result, it was found that these composite filter materials modified with

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GO can interact with the cell membrane of Escherichia coli leading to physical damage to bacterial membrane and inactivation due to the leakage of intracellular matrix (Fig. 12 e).

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However, it was found that the microbiological activity of filtration materials against Escherichia coli can be achieved using nanoparticles as an additive to GO used for the surface

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modification [50,51].

100 90

Cell vvability of bacteria, %

80 70 60 50 40 30

10 0 0.0

1.0

2.0

3.0

4.0

Concentration of GO dispersion, g/dm3

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Fig. 11. The effect of the concentration of the GO aqueous dispersion used for surface modification of

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membranes on the cell viability of Escherichia coli.

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Fig. 12. Surface structure of native membrane (a) and its microbiological activity against Escherichia

CONCLUSIONS

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coli (b); membrane surface modified with 0.5 g/dm3 aqueous dispersion of GO (c, d, e).

In this work the flat sheet polyamide membranes were modified using graphene oxide (GO)

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so as to obtain antibacterial properties. Plasma treatment in a mixture of argon and oxygen (Ar-O2) was used to activate the surface of the tested membranes. As a result of the conducted

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experiments, the process conditions for plasma activation of polyamide membranes were selected allowing GO to be attached on the membrane’s surface. It was found that plasma activation of membranes in the Ar-O2 mixture under the pressure of 1 mbar for 120 seconds and further treatment of the surface with a 0.5 g/dm3 GO aqueous dispersion allow to obtain membranes with high water permeability and disintegrating the cell membrane of Escherichia coli, which in consequence can lead to bacterial death.

Author Contributions Section Anna Kowalik-Klimczak (50%) Ewa Woskowicz (25%) Joanna Kasprzyńska-Gołacka (25%)

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Declaration of interests The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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