Surface Characteristics of a Polyimide Film Treated with a Dielectric Barrier Discharge Plasma

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1 Journal of the Korean Physical Society, Vol. 54, No. 3, March 2009, pp Surface Characteristics of a Polyimide Film Treated with a Dielectric Barrier Discharge Plasma S. M. Kang, W. J. Park and D. H. Yoon School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon (Received 16 June 2008) Polyimide (PI) has many outstanding properties, such as good thermal stability, low dielectric constant, low dissipation factor and inherent surface inertness. The surface characteristics of PI were modied by using a dielectric barrier discharge (DBD) plasma treatment in ambient helium, air and oxygen gas at atmospheric pressure. The surface energy of the PI lms was evaluated using a contact angle analysis according to the sessile-drop method. The plasma-treated surface of the PI lms became hydrophilic. A change in the surface morphology was observed using scanning electron microscopy (SEM). The surface roughness of the plasma-treated PI lms increased compared with that of the untreated lm. In addition, the eects of plasma treatment on the surface chemical characteristics of the PI lms were observed by using X-ray photoelectron spectroscopy (XPS). PACS numbers: Hc, Ps, Mn, b Keywords: Dielectric barrier discharge, Polyimide lm, Surface modication I. INTRODUCTION Polyimide (PI) lms have been used extensively in the elds of aerospace, microelectronics, optoelectronics, composites and ber optics because of their excellent thermal stability, good mechanical properties, low dielectric constant and good chemical resistance [1, 2]. However, their application in industry is restricted because the wetting property of the hydrophobic surface causes poor adhesion between the polymer and other layers. The various surface modications of the polymer that have been studied to overcome the limitation include surface roughening by using chemically active groups induced by plasma treatment, corona discharge or X-ray, laser, ion beam, or ame treatment and chemical treatment by etching in the presence of KOH aqueous solutions [3{10]. Among these various modication methods, plasma treatment has various advantages, such as high eciency and operational simplicity. Plasma treatment takes place only on the surface of the material, without changing its bulk properties. It is also possible to produce various types of plasma, such as oxidative, reductive and inactive ones. The adhesion of a polymer can be explained by its chemical and physical interactions. The surface of a polymer is activated during plasma treatment, which brings about chain scission of existing groups on the surface of the polymer and creates new functional groups such as -OH, -OOH and -NH 2. The surface topography is also changed by ion dhyoon@skku.edu; Fax: bombardment. Appropriate surface treatment enlarges the potential bonding area, which increases the adhesion properties [11,12]. Recent advances in technology have shown that air plasmas can dramatically improve the wettability and adhesion properties of a polymer surface. One of the most exciting technologies to emerge in recent years is dielectric barrier discharge (DBD) plasma processing. In this technology, one or both of a pair of electrodes are covered with a dielectric layer, which limits the amount of charge transported from one electrode surface to the other via single micro-discharges and distributes these microdischarges over the entire electrode area [13]. In this work, we investigated the eects of DBD plasma treatment on the surface properties of PI lms. We studied the physical and the chemical inuence on the surface properties of PI lms after plasma modication in various mixed gas environments. The wetting property of the PI lm surfaces is also discussed. II. EXPERIMENTS AND DISCUSSION The experiments were conducted using commercial PI lms (20 70 mm 2, Du Pont Chemical Co.). The PI lms (scheme 1) were cleaned with isopropyl alcohol in an ultrasonic bath for 30 min and then dried in a vacuum oven at 80 C. The dried PI lms were kept in a vacuum at room temperature before conducting the experiments. The PI lm's surface was subjected to plasma treatment for 90 second by using an atmospheric DBD

2 Surface Characteristics of a Polyimide Film Treated with { S. M. Kang et al Table 1. Surface tension component parameters of the tested liquids, measured at 20 C. Testing Liquids L(mJ/m 2 ) LL (mj/m 2 ) SP L (mj/m 2 ) Water Diiodomethane Ethylene glycol Table 2. Contact angles of the polyimide lms. Testing Liquids non-treated sample He + air + O 2 He + air He + O 2 He Water Diiodomethane Ethylene glycol plasma system. The DBD plasma treatment power was xed at 12 kv and a medium frequency of 30 KHz and the treatment temperature was kept below 35 C. The PI lms were subjected to plasma modication in various mixed gases, such as He, He + O 2, He + air and He + air + O 2, which were named as He, HeO, HA and HAO, respectively. The contact angles of the DBD plasma-treated PI lm surfaces were measured using the sessile drop method with an SEO 300 A unit (Seo Inc., Korea). Deionized water, diiodomethane and ethylene glycol were used as the test liquid, which was dropped onto the PI lm's surface more than ten times in dierent locations at 20 C to obtain more information about the surface free energy of the PI lms before and after DBD plasma treatment. The surface chemistry of the samples was analyzed using X-ray photoelectron spectroscopy (XPS, HP 5950B ESCA spectrometer). The surface morphologies of the PI lms before and after DBD plasma treatment were observed by using scanning electron microscopy (SEM). The surface energy of polymers is more important than the physical and the chemical elements with respect to the resulting mechanical properties of adhesion between polymers. To determine the free energies of surfaces or interfaces, several researchers have developed the theory of non-polar and polar components. According to the theory of polar components, including the acid and base parameters of the surface free energy, the electronacceptor (acid) and the electron-donor (base) characterizations between the polymer surfaces are the most important factors. These parameters provide a real description of the specic surface free energy, which has been applied to various interfacial systems in many areas of surface science. Therefore, we can evaluate the wetting properties of surfaces, such as the hydrophilic and hydrophobic properties, by using contact angle measurement. The concept of surface free energy, rst reported by Fowkes in 1963, is composed of polar and non-polar components as follow as = L + SP ; (1) Fig. 1. Chemical structure of polyimide. where the L and SP are the London dispersive (superscript L) and specic (superscript SP, Debye Keesom of van der Waals, H-bonding, -bonding and other small polar eect) components of the surface free energy of the constitutive elements, respectively. Owens et al. proposed methods to evaluate the surface free energy according to Fowkes' concept [13{15]. Using two wetting liquids with known L L and L SP for equilibrium contact angle measurements, S L and S SP are easily determined by solving [16,17] (1 + cos ) L = 2[L L ) 1=2 + (L SP S SP ) 1=2 ]; (2) where the subscripts L and S represent the liquid and solid states, respectively. The surface free energies for the wetting liquids and their London dispersive and specic components are listed in Table 1. The contact angles for all test liquids largely decreased with DBD plasma treatment in all of the ambient mixed gas conditions, as listed in Table 2. The contact angles of all plasma-treated samples decreased. The wettability property markedly improved for both the non-polar and polar components for the HAO sample. The surface free energy was analyzed to investigate in more detail the surface energy properties of the PI lms with DBD plasma treatment. Figure 2 shows the values of S L and S SP determined from Eq. (2) with the value of the contact angle measurement using deionized water and diiodomethane. The surface free energy of the DBD plasma-treated samples increased with increasing S L and S SP, compared with the plasma-untreated sample. The increase in the S SP value was greater than that of S L, remarkably and was caused by the increased

3 Journal of the Korean Physical Society, Vol. 54, No. 3, March 2009 Fig. 2. Variation of the surface free energy of a DBD plasma-treated polyimide lm. Fig. 3. The O1s/C1s ratio of the DBD surface-modied polyimide lm. Fig. 4. C1s XPS spectra data of the polyimide lm: (a) non-treated, (b) He + air + O 2-treated, (c) He + air-treated, (d) He + O 2-treated and (e) He-treated.

4 Surface Characteristics of a Polyimide Film Treated with { S. M. Kang et al Fig. 5. E ect of DBD plasma treatment on the surface oxygen functionalities on the polyimide lm. formation of oxygen-containing bonds, such as C O and C = O, when the PI lm surface was treated with the DBD plasma. The S SP value of the HAO sample exhibited the largest increase. An XPS analysis was performed to examine the changes in the chemical bonds on the surface of the plasma-treated PI lms. The C1s, N1s and O1s spectra for the PI lms were observed at 285 ev, 404 ev and 532 ev, respectively. Figure 3 shows the O1s/C1s ratio before and after plasma treatment with various mixed gases. When the O1s/C1s ratio was compared between the untreated and the treated PI lms, the value increased dramatically from % for the plasmauntreated sample to % and % for the HA and the HAO samples, respectively. The O1s/C1s ratio for the HeO and the HAO samples increased remarkably with DBD plasma treatment in the oxygen mixed gas condition. To obtain more information about the surface chemical properties of PI lms before and after DBD plasma treatment, we analyzed the C1s core level scan spectra, as shown in Figure 4. The C C, C N, C O and C = O bonds were observed at ev, ev, ev and ev, respectively. The! phenomena was observed for all DBD plasma-treated samples. However, no C N or C O bonds were observed for the DBD plasma-treated samples with ambient He, air mixed gas, ambient He gas. The C N bonds decreased relatively with increasing of C O bonds for the plasma-treated sample with He gas while the C N bonds increased to a relatively high level for the plasma-treated samples with ambient He and air mixed gas because of the preferred reaction with nitrogen from the air. Figure 5 shows the changes in the carbon and the oxygen-containing functionality with DBD plasma treatment for various mixed gases. The C C bonds of the plasma-untreated sample were %, which decreased to % and % for the HeO and the HAO plasma-treated samples, respectively, while C O Fig. 6. SEM micrographs DBD surface treated polyimide lms: (a) non-treated, (b) He + air + O2 -treated, (c) He + air-treated, (d) He + O2 -treated and (e) He-treated. and C = O bonds increased. From the results, we concluded that DBD plasma treatment with various gas mix-

5 Journal of the Korean Physical Society, Vol. 54, No. 3, March 2009 ture conditions is aected by an increase in the oxygencontaining group, which improves the wettability properties of surface for PI lms. The eects of DBD plasma treatment on the morphology of the PI lm surface were investigated. Figure 6 shows the SEM images of the DBD plasma-untreated and plasma-treated PI lms with various mixed gases. The surfaces of all plasma-treated PI lms with various mixed gases were rougher than that of the untreated lm, as shown in Figure 6 (a). The morphology of all the DBD plasma-treated samples was rough compared with the plasma-untreated PI lms. Especially, the surface roughness increased remarkably with increasing oxygen concentration ratio. With HeO, surface cracks were observed because of the higher oxygen concentration in the DBD plasma treatment than in the other samples. However, the HAO sample in the mixed air gas condition had a softer surface than the HeO sample without surface cracks. III. CONCLUSION In conclusion, the surface free energy, chemical properties and morphology of PI lms were modied by using a DBD plasma treatment in various ambient mixed gases. The DBD plasma treatment under various gas mixture conditions was aected by an increase of the oxygencontaining group, which caused wettability properties, such as a hydrophilic surface for the PI lms. The wettability for the PI lm surface was improved because of the increased polar component of the surface free energy induced by the DBD plasma treatment. The oxygencontaining groups of the HAO sample increased remarkably with the surface free energy. The morphology of the DBD plasma-treated samples was rougher than that of the untreated PI sample. Surface cracking was observed for the HeO sample because of the DBD plasma treatment in a higher oxygen concentration. However, the HAO sample treated under a mixed air gas condition was smoother than the HeO sample. REFERENCES [1] L. A. Laius, Polyimide: Thermally Stable Polymer (Consultants Bureau, New York, 1987). [2] W. L. Qu and T. M. Ko, J. Appl. Polym, Sci. 82, 1642 (2001). [3] Q. H. Lu, M. Li, J. Yin, Z. K. Zhu and Z. G. Wang, J, Appl. Polym. Sci. 82, 2739 (2001). [4] J. H. Kim, Y. G. Seol and N.-E. Lee, J. Korean Phys. Soc. 51, 187 (2007). [5] Y. J. Kim, T. J. Byun, S. I. Kim and J. G. Han, J. Korean Phys. Soc. 53, 1401 (2008). [6] H. T. Lokhande, V. S. Thaker and S. R. Shukla, J. Appl. Polym. Sci. 29, 2989 (1984). [7] J. R. Rasmussen, D. E. Bergbreiter and G. M. Whitesides, J. Am. Chem. Soc. 99, 4746 (1997). [8] E. R. Anucci, A. Sandgren, N. Andronova and A. C. Albertsson, J. Appl. Polym. Sci. 82, 1971 (2001). [9] W. J. Lee, Y. B. Kim, K. K. Jee and W. Y. Lee, J. Korean Phys. Soc. 52, 1673 (2008). [10] M. Horie and T. Tamura, J. Appl. Phys. 77, 162 (1995). [11] H. S. Nalwa, Handbook of Thin Film Materials (Harcourt, San Diego, 2002). [12] W. Petasch, E. Rauchle, M. Walker, P. Elsner, Sur. Coat. Technol. 683, 74 (1995). [13] S. Ishikawa, K. Yukimura, K. Matsunaga and T. Maruyama, Surf. Coat. Technol. 130, 56 (2000). [14] F. M. Fowkes, J. Phys. Chem. 67, 2538 (1963). [15] D. K. Owens and R. C. Wendt, J. Appl. Polym. Sci. 13, 1741 (1967). [16] S. Wu, Polymer Interface and Adhesion (Marcel Dekker, Inc., New York, 1982). [17] S. J. Park, W. B. Park and J. R. Lee, Polym. J. 31, 28 (1999)

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