TEKSTİL ve KONFEKSİYON 1 /200 9 

### 45 

## ( REFEREED RESEARCH)



# IMPROVEMENT SURFACE PROPERTIES OF
**POLYPROPYLENE AND POLYESTER FABRICS BY GLOW**
**DISCHARGE PLASMA SYSTEM UNDER ATMOSPHERIC**
**CONDITION**

ATMOSFERİK GLOW DEŞARJ PLAZMA SİSTEMİ İLE POLİPROPİLEN VE POLİESTER KUMAŞLARIN YÜZEY

ÖZELLİKLERİNİN İYİLE ŞTİRİLMESİ

Necla YAMAN Uşak University

, Textile Engineering Departmen , Tu rkey Esen ÖZDOGAN
Ege University, Textile Engineering Department , Tu rkey İ.Cengiz KOCUM Baskent University, Biomedical Engineering D e partment

, Turkey

Hakan AYHAN Mugla Univer

sity, Faculty of Science and Art, Department of Chemistry

, Turkey Tülin ÖKTEM
Ege University

, Textile Engineering Departmen , Tu rkey Necdet SEVENTEKIN Ege University

, Textile Engineering Departmen , Tu rkey necdet.seventekin@ege.edu.tr

**ABSTRACT**

In order t o raise wettability and to improve soil release of polyester (PES) and polypropylene (PP) woven fabr ics, atmospheric pressure plasma were applied. In this study, argon and air plasma were used for modification of PES and PP fabrics. The capillary method and contact angle measurements of plasma treated and untreated textile materials were applied to evaluate the improvement in water uptake of PES and PP fabrics. Chemical changes in the fabric surface after atmospheric plasma treatments were det ermine by
Fo u rier Transform Infrared (FTIR) and XPS. Their surface morphologies were evaluated by SEM

. **Key Words:** Atmospheric p lasma, Polyester, Polyprop y lene, Fiber, Hydrophilicity

**ÖZET**

Atmosferik plasma işlemi uygulanmış poliester (PES) ve polipropilen (PP) dokuma kumaşların kir itici lik özelliği ve ıslanabili r liği incelenmiştir. Bu çalışmada, argon ve hava plazma PES ve PP kumaşların modifikasyonu için kullanılmı ştır. PES ve PP kumaşlar ın hidrofilliklerini değerlendirmek için, işlem görmemiş ve plazma işlemi görmüş materyallere kapilarit e ve temas açısı ölçümleri uygulanmıştır. Plazma işlemi sonunda kumaş yüzeyinde meydana gelen kimyasal değişim Fourier Transfor m Infrare d (FTIR) and XPS ile belirlendi. Yüzey morfolojisi SEM ile değe r lendirilmiştir.

**Anahtar Kelimeler:** Atmosferik p lazma, Poliester, Poliprop i len, Lif, Hidrofillik

Received: 03

. 0 3 .200 8 Accepted: 31

. 0 7 .2008

**1. INTRODUCTION**

The concern in the te xtile industry over reduction of water consumption and
waste

- water treatment in all areas of fiber, yarn and fabric preparation has caused a continuous search for new

non

- aqueous treatment. The plasma treatment of textile materials has been
utilized as a s ubstitution for current wet treatment and pre

- treatment processes. Plasma treatments have been proven effective for increasing particular surface properties of textile materials. The plasma can be produced when a gas at low pressure or atmospheric pressure is submitted to an electric field (1, 2).

In plasma area, many phenomena can occur derived from the plasma/surface interacion of the material. One the main effects of the interaction between active chemical species due to the plasma colliding with a text ile materials is the tearing away of molecules chains, the formation of new functional groups and morphological alterations, like the formation microporosity (3). The treatment gives rise to the formation of free radicals at the surface and further down in the textile materials which react with the excited species in the plasmas. The surface
treatments also lead to a crosslinked skin propagated by recombination of polymer radicals. Chain scission takes place simultaneously with cross

- linking
and oxidation. Small molecule degradation products are constantly removed by evaporation and sputtering, while polymeric scission products remain intermeshed with undergraded polymers and crosslinked networks. The modified depth of polymeric materials thanks to plasma
is between 50

- 500oA (4).

### 46 TEKSTİL ve KONFEKSİYON 1 /200 9

Many studies have already been carried out with low pressure plasma, but atmospheric pressure plasma
treatments would be ideal for the continuous processing of textile materials. It was previously believed that plasmas generated at atmospheric pressure are not uniform or stable; however a research on atmospheric plasma has shown their uniformity, stability and applicability to processing and treatment of textiles. Atmospheric plasma devices and treatments could
be utilized for use in high

- speed continuous processing operation, and when optimized, could replace or increase many current wet

- chemical finishing processes (5, 6).

In this study, PES and PP woven fabrics were modified by atmospheric pressure plasma treatment utilizing air

a nd argon gases and their chemical and morphologic modifications were investigated.

**2. EXPERIMENTAL SET**

**- UP** 

**2.1. Materials**

In this study, 67 g/m 2 PES and 145 g/m 2 PP plain woven fabrics were
used. These fabrics extracted with acetone for 4 hours, thorough ly dried in air. Argon (purity of >99.99) and air (20.9% oxygene, 79.1% nitrogene and relative humidity < 3 ppm) as the process gases were purchased from BOS. Acetone, potassium bichromate, carbon black, liquide paraffin and CCl 4 employed in this work were purchased from Merck Chemical Company.

**2.2. Atmospheric Pressure Plasma**
**Treatment**

For plasma treatment a laboratory scale atmospheric plasma reactor was utilised. The discharge is produced between four electrode (diameter = 17 mm) couples. One of the ele ctrodes in the couple is covered dielectric material, and the inter

- electrode distance is set 2 mm (7). PES and PP fabrics were treated with a power 50,
100 or 130 W and at different time
intervals.

**2.3. Material Characterization**

**2.3.1. Hydrophilicity**

In order to evaluate hydrophilicity of the original and treated PP and PES fabrics, capillary rise and contact angle
measurements of each material were

carr ied out. Capillary rise measurements
were made the method which was described in the Ref. 2. Capillary rise measurement was repeated eight times, and arithmetical mean was taken. Contact angle were measured by using a ganiometric system (Tampere University, in Finland); measurement was repeated ten times,
and the arithmetical mean was taken.

**2.3.2. Soil Res istance** 

Carbon black has been generally used for soil preparations because of their light reflectance properties to simulate soil in a fabric artificially. In our study, the soiling behaviour of the fabrics was investigated according to the procedure desc ribed by Seventekin
and Oktem et.al. (6). To present to soiling data, ΔE values of the fabrics
were collected from the datacolor
Instrument measurement results (Minolta 3600d model spectrophtometer, Turkey).

**2.3.3 Chemical Characterisation**

**FTIR / ATR Analy**  **sis:** (Fourier Transform Infrared Spectroscopy with
Attenuated Total Internal Reflectance mode measurement) The Infrared (IR) spectra of fabrics were determined by
means of a Pe r kin Elmer 100 FTIR spectrometer in ATR reflection mode using a Diamond/zinc sel enide crystal. To ensure reproducible contact between the crystal faces and the fabric, a pressure of 50 kPa was applied to the crystal holder by means of a calibrated torque screw driver. An average of 15 scans using a resolution
4 cm - 1

. **XPS Analysis:** X

- r ay photoelectron spectroscopy was used to monitor the modifications produced in the outermost (5

- 10 nm) po l yester and polypropylene fibres surfaces. In this study, the measurement depth was 7 nm. The fabric samples were analysed using SPCS XPS system with a Mg K  X

- ray source operated at 10 kV and 200 W. The pressure inside analysis
chamber was 10 - 8 to 10 - 9 torr. Survey scans were taken with a pass energy of 48 eV. The peak positions were corrected for charging relative to the
C

- C bond which was assigned a binding energy of 284.5 eV.

0 0,5 1 1,5 2 2,5 3

0 4 20 40 60 4 20 40 60 4 20 40 60

**Exp. Time (s) Capillarity (cm)**  

### Argon **Air**

**100 W 130 W**  **50 W**

**Figure 1.** Capillary rise on PP fabric after plasma treatment at various power and times

0 2 4 6 8 10 12 14 16

0 4 20 40 60 4 20 40 60 4 20 40 60

**Exp. Time (s) Capillarity (cm)**  **Argon Air** 

**100 W 130 W**  **50 W**

**Figure 2.** Capillary rise of PES fabric after plasma treatment at various power and timesTEKSTİL ve KONFEKSİYON 1 /200 9 

### 47

**2.3.4. Morphology**

The microstructure of PP and PES woven fabric before and after plasma were characterized by using SEM a Philips XL30S FEG microscope with digital microscopy imaging.

**3. RESULTS**

**3.1. Evaluation of Hydrophilici ty** 

In this study, to improve the surface properties of PES and PP fabrics, argon and air plasma were carried out at atmospheric pressure. The surface properties were evaluated by measuring capillary rise and contact angle as a function of plasma
treatment time, power and gases. The treatment time and power in both air and argon range between 4

- 60 s and
50

- 130 W, respectively. Fig. 1 and 2 show the warp direction capillary rise results as a function of exposure time and plasma power for PP and PES fabric, re spectivel y . Table 1 shows contact angle results of PP and PES fabric after treatment in air and a r gon plasma.

As shown in Table 1, the contact angle for the PP fabrics was found to change from 105.73o for the untreated sample to the lowest value 81,44o af ter treatment in both discharges, and capillary rise height increased, while contact angles decreased. Figures 2 and Table 1 show that the plasma exposure leaded to similar changes in the PES fabric surfaces with respect to the contact angle: the contact a ngle decreases from 90, 22° for the untreated sample to 39, 23° after treatment in plasmas, and capillary rise height increased. Similar increases in wickability/capillarity were observed by Borcia et. al.(8).

It is shown that the wettability is strongly enhanced by plasma
treatment. When air and a r gon are used in the plasma state for a
treatment time of 1

– 60 second, it incorporates hydrophilic groups such

as

— OH, C=O, C

— O

— O

— , O―C=O etc., predominantly making the surface more hydrophilic. Capillary rise he ight increased unlike contact angles, but a little difference between two plasmas can be seen more clearly from capillarity and contact angle results.

It is shown that air plasma is more efficient in implanting oxygen
functionalities than a r gon plasma. In air plasma, most of the created radicals at the polymer surface will quickly react with an oxygen particle, resulting in an efficient implantation of oxygen functionalities. In contrast, plasma treatment in argon leads to a

cross

- linking reaction in combi nation
with surface oxidation. This crosslinking reaction inhibits the surface oxidation, resulting in a slower incorporation of oxygen functionalities.

When PP and PES are treated in

oxygen

- containing argon plasma, the

cross

- linking and oxidation process occurs in different steps, resulting eventually in an oxidized three

dimensional cross

- linked structure (9). However, the exact mechanism leading to this oxidized cross

- linked structure is not yet described in detail. **3.2. Evaluation of Ageing**

The most se rious problem for plasma treatments is the durability of the treatment. The most probable reason for this has been considered to be “overthrough” or migration of the created p o lar groups into the textile materials (4). The lack of durability has
been attri buted largely to the surface rearrangement of macromoleculer segments which is truly physical but not due to the loss of chemical groups introduced by the surface treatment.
Furthere more the aging seems to depend on the chemical nature of the
substrate. T o determine ageing properties of synthetic textile fabrics after plasma treatment, capillary rise measurement were fulfilled after s even, thirty and one hundred eighty days for samples that were obtained maximum capillarity values (130 W

- 60 s argon and air

plasma). PP and PES fabric results are given Figure 3 and 4, respectively.

As it is shown in the figures, although argon and air plasmas made the surfaces of the PES and PP fabrics hydrophilic, the hydrophilicity decreased with the ageing time, due to
th e rearrangement of hydrophilic functional groups formed by plasma treatments (10). Ageing for the air treated samples were higher than argon treated samples. When inert gases like argon were used for the treatment of polymer surface, ions and UV photons, p resent in the discharge, would break C―C or C―H bonds, leading to the production of carbon radicals. Many more radicals were formed or induced on the PES and PP **Table 1.** Contact angle values of PP and PES fabrics (C.A: Contact Angle, S.D. Std. Dev.)

**PP Fabrics PES Fabrics** 

**Argon Pls. Air Pls.**  **Argon Pls. Air Pls.**  **Power (W) T**  **i me** 

**(sec) C.A (**  ** )**  **S. D. C.A (**  ** )**  **S. D. C.A (**  ** )**  **S. D. C.A (**  ** )**  **S. D.**

**0** 0 105.7 2.47 105.7 2.47 90.22 3.06 90.22 3.06

4 96.24 2.31 98.98 2.54 74.95 3.26 75.66 3.41

20 91.02 2.3 91.32 2.45 71.67 3.2 73.94 3.12

40 87.7 1.97 91.13 2.43 70.54 3.35 73.14 3.27 **50**

60 85.97 1.5 88.38 2.26 54.98 2.95 71.01 3.12

4 94.68 2.45 96.48 2.35 72.88 3.17 65.7 3.21

20 87.69 2.01 89.56 2.15 56.94 3.05 52.98 2.97

40 83.28 1.72 88.28 2.2 52.56 2 .76 48.01 2.28 **100**

60 82.41 1.47 85.2 1.95 51.9 2.46 47.86 1.92

4 93.94 2.25 94.04 2.26 70.43 2.85 55.02 3.03

20 83.69 1.96 88.74 2.13 49.91 2.5 47.34 2.65

40 82.08 1.5 84.24 1.96 48.56 2.56 41.12 2.15 **130**

60 81.44 1.44 83.01 1.4 45.17 1.81 39.23 1.6

### 48 TEKSTİL ve KONFEKSİYON 1 /200 9 surface by argon and these radicals reacted with each other to form crosslinked layers, whic h would be expected to prevent the rearrangement of hydrophilic functional groups formed by plasma treatment (11).

**3.3. Evaluation of Soil Resistance**

Soil release characteristics are especially important for the manufacturers and the end

- users of the fabr ics. Hydrophobic synthetic fibers attract soil to a greater extent than natural fibers because of the development of electrostatic charges on the surface (6).

The ΔE values for the PP and PES fabrics modified by atmospheric argon and air plasmas are given Fig. 5 and 6, respectively. Soil release usually correlates with the hydrophilicity of the fabrics. Activating surfaces are to change their polarity. Polar sur faces
are made more non

- polar to render them repellent to liquids and reduce adhesion of soil particle, non

- polar surfaces will be made more polar to improve water wetting and soil release properties (11).

The relative color intensities of both PES and PP fabrics were increased
thanks to air and a r gon plasma tretmant with increasing treatment time and power.

**3.4. Evaluation of Chemical Characterization** 

**3.4.1 FTIR/ATR Analysis**

Treated PP and PET fibres are measured by FTIR spectrometer in order to investig ate what chemical changing happens at the surface of polymer. The infrared absorption spectras of untreated and plasma

treated PP and PES fabrics are shown in Figure 7 and 8, respectively.

In Figure 7, for the untreated polypropylen fibers, there are two

s trong absorption peaks. Peaks are assigned as follows: C

– H vibration peak in the range of 1460

– 1470 cm - 1

, anti

- symmetric/symmetric CH 2 ve CH 3 peaks in the range of 2820

- 2950 cm - 1

. After the plasma treatments, some new absorption peaks were appeared in Figu re 7 :

- OH stretching vibration
3500

- 3200 cm - 1

, – COOH (carboxylic acid) absorption peak in the range of
1700

– 1750 cm - 1 , C=C non

- saturated double bond conjugated with COO absorb peaks in the range 1630

- 1645

cm - 1 were appeared (12, 13). Functional groups cou ld be generated 0 0,5 1 1,5 2 2,5 3

Right Away One Week Later One Month Later Six Months Later

**Ageing Time Capillarity (cm)**  **untreated 130 W-60 s (Argon)**  **130 W-60 s (Air)**

**Figure 3.** Ageing of plasma treated PP fabrics

0 2 4 6 8 10 12 14 16

Right Away One Week Later One Month Later Six Months Later

**Ageing Time Capillarity (cm)**  **untreated 130 W-60 s (Argon)**  **130 W-60 s (Air)**

**Figure 4.** Ageing of the plasma treated of PES fabrics

0 5 10 15 20 25

0 4 20 40 60 4 20 40 60 4 20 40 60

**Exp. Time (s) Soil Resistence (ΔE)**  **Argon Air** 

**100 W 130 W**  **50 W**

**Figure 5.** Soiling behaviour PP fabrics after atmospheric pressure plasma

0 5 10 15 20 25

0 4 20 40 60 4 20 40 60 4 20 40 60

**Exp. Time (s) Soil Resistance (ΔE)**  **Argon Air** 

**100 W 130 W**  **50 W**

**Figure 6.** Soiling behaviour PES fabrics after atmospheric pressure plasma treatmentTEKSTİL ve KONFEKSİYON 1 /200 9 

### 49

of the fabric surface because intensity of the carbonyl and hydroxyl band increased (13). The functionalization of the surface of the fiber means a higher polarity leading to an increased hydrophilicity.

As can be seen from Fig. 8, contrar y to the new absorption peak appearance of plasma

- treated PP fibre, no new absorption peak come up in the infrared absorption spectra of plasma treated PES compared to the untreated one. The peaks at the wave numbers, 1714, 1250, 1120, 1046 and
726 cm - 1 ar e specific for PES. The three peaks between 2970 and 2846

cm - 1 are the C

– H sp 3 vibration (14). The peak height at 1713 cm - 1 due to C=O absorption shows a slight increase on plasma treatment.

**3.4.2 XPS Analysis**

The XPS show C (1s) and O (1s) peaks, which c haracterise the carbon and oxygen atomic composition in PES and PP fabrics. For more clarity, the chemical composition in terms of C (1s), O (1s) and N (1s) is given in Table 2 and Figure 9 and 10 as function of gases. From this it is clear that the plasma treatment has a significant influence on the PES and
PP surface.

When PES fabric was treated in air plasma for 60 s, a decrease in the C (1s) peak was observed (from 73.3 to 63.3%). At the same time the O (1s) peak increased (from 26.6 to 35.2%).
When PE S fabric was treated in argon plasma for 60 s, a decrease in the C (1s) peak was observed (from 73.3 to 64.8%). At the same time the O (1s) peak increased (from 26.6 to 3 4.1%). The O/C ratio of the untreated, argon and air plasma treated PES increases
as f ollows, respectively: 0.363 < 0.526<0.556. Increasing O/C atomic ratio means that oxygen

- cantaining functional group amount increases.

For the PP fabric, the O/C and N/C ratio of the untreated sample are 6.4 and 0.2 %, respectively. This means
that the un treated PP fabric appears to
contain some contamination or more probably low

- level surface oxidation. After plasma treatment in air and a rgon, the O/C atomic ratio increases to
18.1 and 17.4 % for saturated samples, respectively. These
increases in O/C rat io suggest that

new oxygen

- containing groups are
formed on the fabric surface after treatment with an air or argon plasma.

Furthermore, after plasma treatment,
N/C atomic ratio increases a little because of nitrogen

- containing functional groups or contami nation.

**3.5. Evaluation of Surface Morphology** 

It is known that plasma affects the polymer surface, especially the morphology. SEM images of the untreated, argon and air plasma treated PP and PES fibers are given Fig. 11 and 12, respectively. As seen in fig ures, surface morphology changes significantly after plasma treatment due to etching on the
surfaces of the fiber. **Figure 7.** FTIR results of treated and untreated PP fabrics. a) Untreated, b) a r gon plasma

treated c) air plasma treated

**Figure 8.** FTIR results of treated an d untreated PES fabrics. a) Untreated, b) a r gon plasma treated c) air plasma treated

**Table 2.** Chemical compositions of 130 W

- 60 s argon and130 W

- 60 s air plasma treated

polyester and polypropylene fabrics

Elemental composition (%)

C O N O/C ratio N/C ration

Polypropylene Sample

Untreated 93.8 6.0 0.2 0.064 0.002

Argon treated 84.0 15.2 0.7 0.181 0.008

Air treated 84.3 14.7 1.0 0.174 0.012

Polyester Sample

Untreated 73.3 26.6 0.4 0.363 0.006

Argon treated 64.8 34.1 1.1 0.526 0.017

Air treated 63.3 35.2 1.5 0.556 0.024

### 50 TEKSTİL ve KONFEKSİYON 1 /200 9 Scanning electron microscopy (SEM) image was observed to comprehend the alteration of surface morphology of
treated fabrics . The PP and PES fiber surfaces after a r gon and air plasma treatment are shown in Figures 1 1

– 1 2 with a magnification of 20.000. It can be seen that the surface

- etching process occurs on the surface of argon and air plasma treated fiber.

Figure 11 (a) and 1 2 (a) demonstrates the SEM image of untreated PP and PES fiber, while Figures 11 (b), (c) and
12 (b), c display the SEM images of plasma treated PP and PES fiber with argon and air gases, respectively. Figure 11 (a) and 12 (a) clearly
demonstrate tha t the untreated fibers surface are smooth and free from roughness, indicating that no damage occurs on the fibers surface. However, in Figures 11 (b), (c) and 12 (b), (c) illustrate a change in the f i ber surface morphology. For the PP fiber, when compared with the air plasma treatment, the argon plasma treatment is more effective on the fiber surface. For the PES fiber, when compared with the argon plasma treatment, the air plasma treatment has a more sev ere damage on the fiber surface. This is probably due to the comparatively slow rate of physical etching introduced by

**Figure 11.** SEM images of PP Fabrics. a) Untreated b) Argon tretaed c) Air treated

**Figure 12.** SEM images of PES Fabrics. a) Untreated b) Argon Treated c) Air treated 

## (a) 5 5 0 5 0 0 4 5 0 4 0 0 3 5 0 3 0 0 2 5 0 2 0 0 0 5 0 0 0 1 0 0 0 0 1 5 0 0 0 2 0 0 0 0 2 5 0 0 0 3 0 0 0 0

2 8 9 2 8 8 2 8 7 2 8 6 2 8 5 2 8 4 2 8 3

53 5 534 53 3 532 531 53 0Intensity (%)

B in ding E n ergy (eV ) C -H

C -O / C -N U ntrea ted A rgo n P lasm a
A ir P la sm a

**Figure 9.** XPS results of untreated and treated PP fa brics

5 5 0 5 0 0 4 5 0 4 0 0 3 5 0 3 0 0 2 5 0 0 5 0 0 0 1 0 0 0 0 1 5 0 0 0 2 0 0 0 0 2 5 0 0 0 3 0 0 0 0Intensity (%)

B in d in g E n e rg y (e V ) **U n tre a te d A rg o n p la s m a**  **A ir p la s m a C**  **-H**

**C -O** 
**C -N** 

**C O O**

**Figure 10.** XPS results of untreated and treated PES fabrics

**(a) (**  **b )**  **( c**  **)**

**(a) (**  **b )**  **( c**  **)**TEKSTİL ve KONFEKSİYON 1 /200 9 

### 51

the argon plasma gas (15). Granules, microcraters, and ripple

- like structures of submicrometer size are observed on the air plasma

- treated surface (Fig. 11 (c)) (16). In summary, plasma
trea tment with air gas is more efficient because air has oxygene molecules. It also signifies that a stronger porous surface effect is created on the air plasma

- treated PES fibers.

**4. CONCLUSION**

In this paper, PP and PES fabrics were plasma

- modified using a di electric barrier discharge in air and argon at atmospheric pressure. The results showed that all of contact angle of PP and PES surfaces decreased, and their capillary rise height increased with plasma treatment, which means the surface hydrophilicity of a ll material surfaces have been improved. Air plasma treatment was more effective in reducing the contact angle due to the fast reaction between created radicals at the polymer surface and oxygen species. In contrast, in

a r gon, cross

- linking competes with

s urface oxidation, resulting in lower modification efficiency.

The modified surface was not stable with time, and undergoes rearrangement of the modified surface layers, leading to the incorporation of some of the functional groups within the surface layer s. Therefore, to characterize and use these surfaces,
their time

- dependent nature has to be
taken into account.

Soil release usually correlates with the hydrophilicity of the fabrics. It can be roughly estimated that the better is the soil release, the be tter is the hydrophilicity of the fabrics. The XPS and ATR

- FTIR results showed that the percentage of oxygen atom in these samples increases and it consisted with the contact angle measurement. Evaluating SEM results
of PES and PP surface with their

conta ct angle datas, it was found that the increasing of surface roughness in micron scale can also improve hydrophilicity, besides the contribution of the rising up of percentage of the oxygene atom.

Therefore, it can be concluded that atmospheric pressure col d plasma could be effectively and safely used to improve hydrophilicity of the polymeric substrates without incurring high cost or creating environmental pollution.

**ACKNOWLEDGEMENTS:** This study was funded by the TUBİTAK

- Textile Research Center, İzmir

- TUR KEY

.

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karar vermişlerdir.