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2764. Cramm, R.H., “The influence of processing conditions on the hot tack of polyethylene extrusion coatings,” in 1988 Polymers, Laminations and Coatings Conference Proceedings, 35-39, TAPPI Press, 1988 (also in TAPPI J., V. 72, p. 185-189, Mar 1989).

1611. Erbil, H.Y., and R.A. Meric, “Determination of surface free energy components of polymers from contact angle data using nonlinear programming methods,” Colloids and Surfaces, 33, 85-97, (1988) (also in Interfaces in Polymer, Ceramic, and Metal Matrix Composites, H. Ishida, ed., Elsevier, 1988, p. 765-772).

1610. Klemberg-Sapieha, Y., A. Migdal, M.R. Wertheimer, and H.P. Schreiber, “Application of plasma treatments to the control of properties in polymer systems,” in Interfaces in Polymer, Ceramic, and Metal Matrix Composites, H. Ishida, ed., 583-594, Elsevier, 1988.

857. Zhanxun, C., C. Jie, and W. Zhizhong, “ESCA characterization of plasma-polymerized tetrafluoroethylene,” in Advances in Low-Temperature Plasma Chemistry, Technology, Applications, Boenig, H.V., ph.d, ed., 265-274, Technomic, 1988.

856. de Mendez, M., J.C. Boeda, G. Legeay, J.C. Brosse, and P. Simon, “Low temperature plasma modification of polysiloxanes,” in Advances in Low-Temperature Plasma Chemistry, Technology, Applications, Boenig, H.V., ed., 229-242, Technomic, 1988.

654. van Damme, H.S., A.H. Hogt, and J. Feijen, “Surface mobility and structural transitions of poly(n-alkyl methacrylates) probed by dynamic contact angle measurement,” in Polymer Surface Dynamics, Andrade, J.D., ed., 89-110, Plenum Press, 1988.

650. Owen, M.J., T.M. Gentle, T. Orbeck, and D.E. Williams, “Dynamic wettability of hydrophobic polymers,” in Polymer Surface Dynamics, Andrade, J.D., ed., 101-110, Plenum Press, 1988.

647. Marchant, R.E., C.J. Chou, and C. Khoo, “Effect of nitrogen RF plasma on the properties of polypropylene,” in Plasma Polymerization and Plasma Treatment of Polymers, Yasuda, H.K., ed., 126-138, John Wiley & Sons, 1988.

643. Lee, J.H., and J.D. Andrade, “Surface properties of aqueous PEO/PPO block block copolymer surfactants,” in Polymer Surface Dynamics, Andrade, J.D., ed., 119-136, Plenum Press, 1988.

642. Lavielle, L., “Orientation phenomena at polymer - water interfaces,” in Polymer Surface Dynamics, Andrade, J.D., ed., 45-66, Plenum Press, 1988.

641. Jhon, M.S., and S.H. Yuk, “Contact angles at polymer - water interface; temperature dependence and induced deformation,” in Polymer Surface Dynamics, Andrade, J.D., ed., 25-44, Plenum Press, 1988.

640. Iriyama, Y., and H. Yasuda, “Plasma treatment and plasma polymerization for surface modification of flexible poly(vinyl chloride),” in Plasma Polymerization and Plasma Treatment of Polymers, Yasuda, H.K., ed., 97-124, John Wiley & Sons, 1988.

639. Hoffman, A.S., “Biomedical applications of plasma gas discharge processes,” in Plasma Polymerization and Plasma Treatment of Polymers, Yasuda, H.K., ed., 251-267, John Wiley & Sons, 1988.

627. Chaney, R., and G. Barth, “An ESCA study on the x-ray induced changes in polymeric materials,” in Polymer Surface Dynamics, Andrade, J.D., ed., 171-178, Plenum Press, 1988.

Electron Spectroscopy for Chemical Analysis (ESCA) is generally considered to be a non-destructive analytical technique as compared to e.g., SIMS and Auger spectroscopy. In fact, there have appeared only a few reports in the literature where soft X-ray induced spectral changes were noted. These studies have recently been reviewed by Storp. Several of these studies have been carried out with non-monochromatic X-ray sources which typically expose a sample surface with a flux of high kinetic energy electrons and thermal radiation. As pointed out by Storp, it is not entirely clear whether or not the reported changes can be therefore considered as uniquely caused by X-ray photons. Wheeler and Pepper have published a detailed beam damage study on polytetrafluoroethylene (Teflon) using a non-monochromatic X-ray source. The authors provided convincing evidence that the detected fluorine depletion of the surface is indeed caused by X-rays rather than electron bombardment. We wish to report ESCA experiment on Teflon and several other polymeric materials using a spectrometer with a monochromatic Al Kα X-ray source. Due to the physical separation between source and sample an unambiguous differentiation between X-ray vs. electron induced damage can be obtained.

604. Yasuda, T., K. Yoshida, T. Okuno, and H.K. Yasuda, “A study of surface dynamics of polymers, III. Surface dynamic stabilization by plasma polymerization,” J. Polymer Science Part B: Polymer Physics, 26, 2061-2074, (1988).

As demonstrated in Part II of this series of studies, the hydrophobic character of CF4 plasma-treated Nylon 6 and poly(ethylene terephthalate) (PET) decay with time of water immersion, and the rate of decay can be used as a measure for the surface mobility of (substrate) polymers. The same method of using fluorine-containing moieties introduced by CF4 plasma treatment as surface labeling is applied to investigate the influence of a thin layer of plasma polymer of methane applied onto the surface of those polymers. An ultrathin layer of plasma polymer provides a barrier to the rotational and diffusional migration of the introduced chemical moieties from the surface into the bulk of the film. The influence of operational parameters of plasma polymerization on the surface dynamic stability are examined by measuring the decay rate constants for (subsequently) CF4 plasma-treated samples. The rate constant was found to decrease sharply with increasing value of plasma energy input manifested by J/kg monomer, and no decay was observed as the energy input reached a threshold value (about 6.5 GJ/kg for PET, about 7.0 GJ/kg for Nylon 6), indicating that unperturbable surfaces can be created by means of plasma polymerization.

589. Vavruch, I., “On the relation between surface energy, internal pressure and molar volume in pure fluids,” Colloids and Surfaces, 30, 405+, (1988).

518. Lekan, S.F., “Corona treatment as an adhesion promoter for UV/EB curable coatings,” in RadTech 88 Proceedings, RadTech, 1988.

517. Lekan, S.F., “Surface treatment of polyolefins for decorating and adhesive bonding,” in RadTech 88 Proceedings, RadTech, 1988.

466. Grant, J.L., D.S. Dunn, and D.J. McClure, “Argon and oxygen sputter etching of polystyrene, polypropylene, and poly(ethylene terephthalate) thin films,” J. Vacuum Science and Technology, A6, 2213-2220, (1988).

Surface chemical modification of polymer thin films induced by sputter etching was studied by x‐ray photoelectron spectroscopy (XPS) and infrared reflection–absorption spectroscopy (IRRAS). The polymers studied were polystyrene, polypropylene, and poly(ethylene terephthalate) (PET). Oxygen and argon sputter etching of these polymers causes surface oxidation and possibly crosslinking; trends in polymer oxidation can be correlated with the etchant gas, etch power, and initial material properties. For polystyrene and polypropylene, the predominant new functionalities formed are CDouble BondO and CSingle BondO groups; the breadth of the infrared absorption bands suggests that many different types of these groups exist. For PET, the predominant damage mechanism is crosslinking, with only a slight degree of oxidation resulting from oxygen sputter etching. This work suggests that the information provided by XPS and IRRAS is highly complimentary and will be useful in future studies of polymer functionalization and derivatization.

465. Golander, C.-G., and B.-A. Sultan, “Surface modification of polyethylene to improve its adhesion to aluminum,” J. Adhesion Science and Technology, 2, 125-135, (1988).

The effects of surface modification of polyethylene (PE) and aluminum on the adhesion strength have been investigated. PE was modified by KMnO4/H2SO4 treatment followed by adsorption of different cations, Ca2+, Ba2+, and Zn2+. The aluminum surface was treated with alkali and was also modified by adsorption of titanates. The surfaces were characterized by means of multiple internal reflection (MIR) IR and ESCA. The adhesion strength was measured by the T-peel test. Both ESCA and MIR analyses show the presence of hydroxyl, carbonyl, ester, and carboxyl groups on the KMnO4/H2SO4-treated PE surface. In addition, sulfate and sulfonate groups are present. The sulfonate groups are apparently localized in crevices extending beneath the ESCA sampling depth of 50 A. Vinylidene groups are also present on the surface. Cation adsorption on the oxidized PE surface seems to be determined by the solubility constant of the corresponding sulfate salts and is in the order Ba2+ > Ca2+ > Zn2+. Adsorption of Ca2+ and Ba2+ increases the relative concentration of oxygen-containing groups on the KMnO4/H2SO4-treated surface. A further increase is seen after annealing. KMnO4/H2SO4 treatment almost doubled the adhesion strength of PE to aluminum. Ca2+ adsorption on the surface prior to lamination increased the adhesion strength nearly three times and caused cohesive failure in the T-peel test. However, when Zn2+ was adsorbed, the adhesion strength decreased drastically. Alkaline treatment of the aluminum surface had only a minor effect on adhesion. The chemical structure of the adsorbed titanates has a great influence on the adhesion strength.

435. Chang, C.-A., “Interface interactions relevant to packaging techology,” Thin Solid Films, 166, 97, (1988).

433. Chae, C., “Characterization of surfaces by contact angle goniometry: effect of curvature on contact angle (PhD thesis),” Univ. of Lowell, 1988.

426. Boenig, H.V., ed., Advances in Low-Temperature Plasma Chemistry, Technology, Applications, Technomic, 1988.

412. Andrade, J.D., ed., Polymer Surface Dynamics, Plenum Press, 1988.

399. Yasuda, T., T. Okuno, K. Yoshida, and H.K. Yasuda, “A study of surface dynamics of polymers, II. Investigation by plasma surface implantation of fluorine-containing moieties,” J. Polymer Science Part B: Polymer Physics, 26, 1781-1794, (1988).

Macromolecules at the surface of a polymeric solid have considerable mobility, and the specific arrangement of functional groups of macromolecules at the surface is dictated by the environmental conditions in which the surface is placed. Consequently, the change of environmental conditions, such as immersion in water or placement in a biological surrounding, could cause a cosiderable degree of change in the surface characteristics of a polymer from those evaluated in the laboratory against ambient air. The mobile nature of a polymer surface can be investigated by surface-implanting fluorine-containing moieties, mainly—CF3, by the plasma implantation technique and following the disappearance and reappearance of fluorine atoms on the surface. The disappearance rates (based on the immersion time in water at room temperature) of ESCA F1s signals, the decay rates of (advancing) contact angle of water, and the recovery of these values on heat treatment of water-immersed samples were measured as a function of crystallinity of polymer samples (at three levels of crystallinity) for poly(ethylene terephthalate) and nylon 6.

373. van Oss, C.J., M.K. Chaudhury, and R.J. Good, “Interfacial Lifschitz-van der Waals and polar interactions in macroscopic systems,” Chemical Review, 88, 927-941, (1988).

apolar interactions in macroscopic systems, cell separation methods. the nature of the interaction between antigens and antibodies. and physicochemical and immunochemical cell surface characterization.

253. Nakayama, Y., T. Takahagi, F. Soeda, K. Hataga, et al, “XPS analysis of NH3 plasma-treated polystyrene films utilizing gas phase chemical modification,” J. Polymer Science Part A: Polymer Chemistry, 26, 559-572, (1988).

Gas phase chemical modification (GCM) is found to be more preferable as a pretreatment for the XPS surface analysis of polymer materials than the conventional liquid phase treatment because it can circumvent problems such as solvent contamination and swelling. We have tried the quantification of the surface composition successfully by estimating the yield of the reaction from model samples. GCM was then applied to correlate the surface composition of NH3 plasma-treated polystyrene films with their cell-affinity. The amount of primary-amine and that of carboxylic acid were directly determined by GCM. Although the amount of primary-amine, 15–20% of total nitrogen, did not depend on the treatment intensity, the total amine content for the treated samples increased with the plasma treatment intensity. The quantity of carboxylic acid generated was found to be very small. All treated samples had better cell-affinity than the control. The sample N2 (of medium treatment) showed the best cell-affinity. The most strongly treated sample N3, with larger amine content than N2, showed worse cell-affinity because of the interference by the sputtered SiO2 on the surface.

234. Matienzo, L.J., F. Emmi, F.D. Egitto, et al, “Surface composition and distribution of fluorine in plasma-fluorinated polyimide,” J. Vacuum Science and Technology, A6, 950-953, (1988).

Surface composition, fluorine distribution, and morphology were determined for polyimide films modified downstream from microwave plasmas containing CF4/O2. Complementary analytical techniques including x‐ray photoelectron spectroscopy, Rutherford backscattering spectroscopy, and scanning electron microscopy yielded a more complete understanding of polyimide fluorination and subsequent etching of the modified film. Depth of fluorination increased nonlinearly with treatment time for films exposed downstream from a CF4‐rich plasma. Exposure downstream from an O2‐rich plasma resulted in a reduction of thickness in both the fluorinated layer and the unmodified polyimide during etching. Finally, a model for fluorination of polyimide and subsequent removal is proposed.

233. Mascia, L., G.E. Carr, and P. Kember, “Plasma treatment of PTFE: effects of processing parameters on bonding properties,” Plastics and Rubber Processing and Applications, 9, 133-140, (1988).

173. Iwata, H., A. Kishada, M. Suzuki, Y. Hata, and Y. Ikada, “Oxidation of polyethylene surface by corona discharge and subsequent graft polymerization,” J. Polymer Science Part A: Polymer Chemistry, 26, 3309-3322, (1988).

Oxidation of a polyethylene (PE) surface by corona discharge and the subsequent graft polymerization of acrylamide (AAm) were studied. The maximum amount of peroxides introduced by corona treatment at a voltage of 15 kV was about 2.3 × 10−9 mol cm−2. The decomposition rate of peroxide and the dependence of graft amount on the storage period of the corona-treated PE films showed that there were several kinds of peroxides, the labile one being mainly responsible for the initiation of graft polymerization. When the corona-treated film was brought into contact with a deaerated aqueous solution of AAm, graft polymerization took place more strongly with the treatment time, but was reduced after passing a maximum. Although the x-ray photoelectron spectroscopic analyses of the corona-treated PE films showed homogeneous oxidation of the outer polymer surface by corona discharge, optical microscopy on the cross section of the grafted film revealed the graft polymerization to be limited to a very thin surface region.

136. Golub, M.A., T. Wydeven, and R.D. Cormia, “ESCA study of Kapton exposed to atomic oxygen in low Earth orbit or downstream from a radio-frequency oxygen plasma,” Polymer Communications, 29, 285-288, (1988).

The ESCA spectra of Kapton polyimide film exposed to atomic oxygen O(3P), either in low earth orbit (LEO) on the STS-8 Space Shuttle or downstream from a radio-frequency oxygen plasma, were compared. The major difference in surface chemistry induced by the two types of exposure to O(3P), both of which caused surface recession (etching), was a much larger uptake of oxygen by Kapton etched in the O2 plasma than in LEO. This difference is attributed to the presence of molecular oxygen in the plasma reactor and its absence in LEO: in the former case, O2 can react with radicals generated in the Kapton molecule as it etches, become incorporated in the etched polymer, and thereby yield a higher steady-state ‘surface oxidation’ level than in LEO.

86. Dryden, P., J.H. Lee, J.M. Park, and J.D. Andrade, “Modeling of the Wilhelmy contact angle method with practical sample geometries,” in Polymer Surface Dynamics, 9-24, Plenum Press, 1988.

45. Burrell, M.C., and J.J. Chera, “Surface analysis of BPA-polycarbonate/poly(butylene terephthalate) blends by x-ray photoelectron spectroscopy,” Applied Surface Science, 35, 110-120, (1988).

X-ray photoelectron spectroscopy is used to measure the surface composition of polycarbonate/ poly(butylene terephthalate) blends. The blend surface is enriched in PC compared to the bulk, with the surface PC/PBT ratio equal to about 1.6 times to bulk formation. For blends containing an impact modifier as a third component, the XPS spectra of the molded surface indicates that no impact modifier is present within the XPS sampling depth. A spectral simulation scheme improves the accuracy of the computed PC/PBT ratio over conventional data reduction schemes involving curve fitting.

357. Strobel, M., P.A. Thomas, and C.S. Lyons, “Plasma fluorination of polystyrene,” J. Polymer Science Part A: Polymer Chemistry, 25, 3343-3348, (Dec 1987).

ESCA and contact-angle measurements were used to characterize the surfaces of polystyrene films exposed to SF6, CF4, and C2F6 plasmas. SF6 plasmas cause loss of aromaticity in the polystyrene surface region via saturation of the phenyl ring and/or carbon-bond breakage and subsequent fluorination. C2F6 plasmas graft CFx radicals directly to the polystyrene surface without necessarily destroying the aromaticity of the polymer. CF4 plasmas appear to be intermediate in character between SF6 and C2F6 plasmas.

459. Frederickson, G.H., “Surface ordering phenomena in block copolymer melts,” Macromolecules, 20, 2535-2542, (Oct 1987).

A mean field theory is presented to describe surface ordering phenomena in diblock copolymers near the microphase separation transition (MST). We consider a near-symmetric diblock melt in the vicinity of a solid wall or free surface, such as a film-air interface. The surface is allowed to modify the Flory interaction parameter and the chemical potential in the adjacent copolymer layer. The composition profile normal to the surface is investigated both above and below the MST. In contrast to the surface critical behavior of binary fluids or polymer blends, we find interesting oscillatory profiles in copolymers that arise from the connectivity of the blocks. These composition profiles might be amenable to study by ellipsometry, by evanascent wave-induced fluorescence, or by scattering techniques. Wetting and other surface phenomena and transitions in block copolymers are briefly discussed.

1460. Mascia, L., G.E. Carr, and P. Kember, “Adhesion enhancement of PTFE by plasma treatment,” in Adhesion '87, 22/1-22/19, Sep 1987.

94. Dick, F., “Apparatus and methods for determining the wettability of various substrates,” U.S. Patent 4694685, Sep 1987.

2790. Tietje, A., “Fifteen years of ozone treatment in extrusion coating,” in 1987 Polymers, Laminations and Coatings Conference Proceedings, 221-224, TAPPI Press, Aug 1987.

1393. Glover, J.H., “Slip migration in extrusion coatings of LDPE,” in 1987 Polymers, Laminations and Coatings Conference Proceedings, 231, TAPPI Press, Aug 1987.

582. Thompson, K., “Flame surface treatment - new perspectives,” in 1987 Polymers, Laminations and Coatings Conference Proceedings, 213-216, TAPPI Press, Aug 1987.


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