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1743. Egitto, F.D., L.J. Matienzo, K.J. Blackwell, and A.R. Knoll, “Oxygen plasma modification of polyimide webs: Effect of ion bombardment on metal adhesion,” J. Adhesion Science and Technology, 8, 411-433, (1994) (also in Plasma Surface Modification of Polymers: Relevance to Adhesion, M Strobel, C.S. Lyons, and K.L. Mittal, eds., p. 231-254, VSP, Oct 1994).

Webs of Kapton 200-H and Upilex-S polyimide films were treated using oxygen plasma prior to sequential sputter deposition of chromium and copper in a roll metallization system. Two plasma system configurations were employed for treatment. In one configuration, the sample traveled downstream from a microwave plasma; in the other, the web moved through a DC-generated glow discharge. For the DC-glow treatment, the potential difference between the plasma and the web, Φf, and relative ion densities, n+, were measured at various values of chamber pressure and DC power using a Langmuir probe. Although samples treated downstream from the microwave plasma were not subjected to bombardment by energetic ions, Φf for the DC-glow operating conditions was between 5 and 13 eV. For both films, advancing DI water contact angles of less than 20° were achieved using both modes of treatment. Contact angles for untreated films were greater than 60°. However, 90° peel tests yielded values of 15 to 20 g/mm for microwave plasma treatments and 40 to 60 g/mm for DC-glow treatment. Peel values for untreated Kapton and Upilex films were about 25 g/mm. High-resolution X-ray photoelectron spectroscopy in the C1s region for Kapton film surfaces treated downstream from the microwave plasma showed increases in carbonyl groups, with concentrations inversely proportional to web speed. In contrast, DC-glow modification was due mainly to formation of carboxylates with a small increase in carbonyl component. It is proposed that treatment downstream from the microwave plasma results in formation of a weak boundary layer at the polyimide surface. Ion bombardment occurring in the DC-plasma configuration results in relatively more crosslinking at the polymer surface. Furthermore, adhesion between the sputter-deposited chromium and the DC-glow modified polyimide improved with increasing values of Φfn+.

1481. Ghali, K., B. Jones, and J. Tracy, “Experimental techniques for measuring parameters describing wetting and wicking in fabrics,” Textile Research J., 64, 106-111, (1994).

Once capillary pressure and permeability are determined for saturations ranging from near zero to 100%, liquid transport related to both wicking and wetting behavior can be described by Darcy's equation. The purpose of the work reported here is to assess and develop experimental techniques that allow capillary pressure and per meability to be measured over a wide range of saturations. Cotton and polypropylene fabrics are the test materials. Capillary pressure head is measured as a function of saturation for cotton and polypropylene fabric samples using the column test, and permeability is measured as a function of saturation using the siphon test. The siphon test works for cotton but not for polypropylene. A new method using a transient measurement technique is developed to determine the permeability of both samples as a function of saturation; it works well for both samples.

1447. Gengenbach, T.R., X. Xie, R.C. Chatelier, and H.J. Griesser, “Evolution of the surface composition and topography of perfluorinated polymers following ammonia-plasma treatment,” J. Adhesion Science and Technology, 8, 305-328, (1994) (also in Plasma Surface Modification of Polymers: Relevance to Adhesion, M. Strobel, C.S. Lyons, and K.L. Mittal, eds., p. 123-146, VSP, Oct 1994).

Treatment of fluorinated ethylene propylene (FEP) and polytetrafluoroethylene (PTFE) in ammonia plasmas produced surfaces with very high wettability by water, but on storage in air at ambient temperature, the air/water contact angles increased markedly. The evolution of the surface composition and topography was studied by angle-dependent X-ray photoelectron spectroscopy (XPS), derivatization of amine groups with fluorescein isothiocyanate, scanning tunelling microscopy (STM), and atomic force microscopy (AFM). XPS demonstrated a continuous increase in the oxygen content over periods of weeks; this was assigned to oxidation of trapped radicals and subsequent secondary reactions. In addition, the fluorine content also changed markedly on storage; the XPS fluorine signal suggested that there was a substantial amount of fluoride in the freshly treated surfaces, and this component disappeared rapidly on storage. STM and AFM showed no changes in topography with aging but suggested surface hardening on plasma treatment. The events following treatment of FEP and PTFE in ammonia plasmas are not adequately described by a model involving plasma-induced, instantaneous chemical modification followed by surface restructuring; the surface and sub-surface compositions evolve over a period of several weeks due to the occurrence of oxidative reactions, and these chemical changes interact with the physical process of surface restructuring.

1445. Mathieson, I., D.M. Brewis, I. Sutherland, and R.A. Cayless, “Pretreatments of fluoropolymers,” J. Adhesion, 46, 49-56, (1994).

In the present study the mechanisms and effectiveness of various pretreatments for fluoropolymers were studied. The pretreatments were “Tetra-Etch,” various plasmas, flame and potassium hydroxide. “Tetra-Etch” was found to be much more reactive than potassium hydroxide (KOH) towards fluoropolymers. The plasma treatment of PTFE showed that it was possible to get substantial increases in adhesion with little or no chemical change to the polymer. However, to obtain large increases in adhesion it may be necessary to modify PTFE chemically as with “Tetra-Etch.” Consideration of the bonding of these fluoropolymers shows that sharp interfaces between these substrates and adhesives do not exist.

1444. Shi, M.K., A. Selmani, L. Martinu, E. Sacher, M.R. Wertheimer, and A. Yelon, “Fluoropolymer surface modification for enhanced evaporated metal adhesion,” J. Adhesion Science and Technology, 8, 1129-1141, (1994).

Adhesion of evaporated Cu to Teflon PFA (polytetrafluoroethylene-co-perfluoroalkoxy vinyl ether) was greatly enhanced by plasma pretreatment. The efficiency of the treatment decreased in the following order: N2 > O2 > (N2 + H2) > (O2 + H2) > H2. X-ray photoelectron spectroscopy (XPS) showed the loss of fluorine and the incorporation of oxygen and nitrogen at the polymer surface. Among the gases, H2 was found to be the most efficient for fluorine elimination, and (N2 + H2) for surface functionalization. Based on this investigation, it is proposed that Cu reacts with both oxygen and nitrogen to form, respectively, Cu-O and Cu-N bonds at the interface but no reaction occurs with carbon and fluorine. While greater enhancement in polymer surface wettability and stronger interfacial reactions can account for the higher performance of N2 over O2 in improving adhesion, these effects cannot explain the lower efficiency of H2. Several possibilities are discussed, including surface cleaning, oxygen incorporation and the formation of weak boundary layers.

1307. Moy, E., F.Y.H. Lin, Z. Policova, and A.W. Neumann, “Contact angle studies of the surface properties of covalently bonded poly-L-lysine to surfaces treated by glow-discharge,” Colloid and Polymer Science, 272, 1245-1251, (1994).

Contact angle data, measured by using a sessile drop arrangement in conjunction with Axisymmetric Drop Shape Analysis-contact Diameter (ADSA-CD), were used to quantify the effects of ammonia gas plasma treatment on the surface properties of previously untreated polystyrene surfaces. The surface tension of treated polystyrene samples is considerably higher than that of untreated samples. The increase in surface tension following plasma treatment is attributed to the addition of amine groups to the surface.

Next, conformational changes following the attachment of poly-L-lysine to the untreated samples by simple adsorption and plasma treated samples by covalent bonding were investigated. Surface tension values obtained from contact angle data indicate that conformational changes to poly-L-lysine occur in both cases, because these values are lower than the surface tension of poly-L-lysine in solution. However, contact angle data show that covalently bonded poly-L-lysine undergoes less conformational changes than simply adsorbed poly-L-lysine.

1306. Kwok, D.Y., D. Li, and A.W. Neumann, “Evaluation of the Lifshitz-van der Waals/acid-base approach to determine interfacial tensions,” Langmuir, 10, 1323-1328, (1994).

1305. Kwok, D.Y., D. Li, and A.W. Neumann, “Fowkes' surface tension components approach revisited,” Colloids and Surfaces A: Physicochemical and Engineering Aspects, 89, 181-191, (1994).

By comparing the number of degrees of freedom obtained from the phase rule for capillary systems, the Fowkes surface tension component approach for interfacial tensions is shown to require more degrees of freedom than are available for a two-component solid—liquid—vapour system. Only in a special case has the Fowkes approach two degrees of freedom: a dispersive liquid on a dispersive solid, suggesting that there are no surface tension components. Experimental results suggest that the Fowkes component approach does not describe physical reality; only the liquid and solid surface tensions, γ1v and γsv, are operative in the two-component solid—liquid—vapour system. Generalization of the Fowkes component approach, of course, will increase the number of independent variables and hence definitely require more degrees of freedom than are available.

The number of degrees of freedom of the equation of state for interfacial tensions is shown to agree with that predicted from the phase rule for capillary systems as well as with experimental results. By using the empirical form of the equation of state, essentially constant solid tensions, γsv, are obtained from a variety of dispersive and non-dispersive liquids for three solid surfaces: fluorocarbon (FC721), Teflon (FEP) and poly(ethylene terephthalate) (PET).

953. Moore, M.J., “Surface energy measurements and their application to rubber-to-metal bonding,” Presented at The 145th Meeting of the Rubber Division of the American Chemical Society, 1994.

853. Bergbreiter, D.E., “New synthetic methodology for grafting at polymer surfaces,” in Chemically Modified Surfaces, Pesek, J.J. and I.E. Leigh, eds., 24-40, Royal Society of Chemistry, 1994.

835. Collaud, M., S. Nowak, O.M. Kuttel, and L. Schlapbach, “Enhancement of the sticking coefficient of Mg on polypropylene by in situ ECR-RF Ar and N2 plasma treatments,” J. Adhesion Science and Technology, 8, 435-453, (1994) (also in Plasma Surface Modification of Polymers: Relevance to Adhesion, M. Strobel, C.S. Lyons, and K.L. Mittal, eds., p. 255-274, VSP, Oct 1994).

A study of the sticking coefficient of Mg vapour on in situ Ar and N2 plasma-treated polypropylene (PP) is presented. After exposure of the pretreated sample to a determined amount of Mg vapour, X-ray photoelectron spectroscopy (XPS) allows measurement of the adhered Mg amount at the polymer surface and the chemical nature of the interface. The sticking coefficient on an as-received sample is zero and is increased to several tenths depending on the pretreatment conditions, namely the nature and the pressure of the neutral gas, the treatment time, and the applied RF-bias. Relations between the plasma parameters, the XPS measured surface state before the metallization, and the sticking coefficient are investigated.

827. Clouet, F., M.K. Shi, R. Prat, Y. Holl, P. Marie, et al, “Multitechnique study of hexatriacontane surfaces modified by argon and oxygen RF plasmas: effect of treatment time and funtionalization, and comparison with HDPE,” J. Adhesion Science and Technology, 8, 329-361, (1994) (also in Plasma Surface Modification of Polymers: Relevance to Adhesion, M. Strobel, C.S. Lyons, and K.L. Mittal, eds., p. 65-98, VSP, Oct 1994).

Hexatriacontane (C36H74) has been used as a model molecule for the study of the surface modifications of high-density polyethylene (HDPE) in argon and oxygen radio-frequency (RF) plasmas. The combination of static secondary ion mass spectrometry (SIMS), ion scattering spectroscopy (ISS), X-ray photoelectron spectroscopy (XPS), and contact angle measurements has constituted a powerful method for the investigation of the surface modifications induced by the plasma treatments. The surface degradation and functionalization are shown to depend on both the nature of the treated material and the nature of the plasma atmosphere. The SSIMS results obtained on plasma-modified hexatriacontane and HDPE are compared in order to identify the nature of the functionalities present at the plasma-treated surfaces. Finally, plasma treatment 18O atmosphere was performed on HDPE, C36H74, and polystyrene (PS). In that case, the isotopic specificity of both ISS and SIMS allowed the determination of the relative concentrations of 16O and 18O in relation to the probed depth and plasma atmosphere.

653. Sugita, K., “Wettability and adhesion of polymer surfaces,” Nippon Gomu Kyokaishi, 60, 246+, (1994) (also in International Polymer Science and Technology, Vol. 14, p. 38-46 (Sep 1994)).

457. Miller, A., “Unit operation 1 - surface treatment of substrates,” in Converting for Flexible Packaging, 23-34, Technomic, 1994.

819. Lee, K.-W., “Modification of polyimide morphology: relationship between modification depth and adhesion strength,” J. Adhesion Science and Technology, 8, 1077-1092, (1994) (also in Polymer Surface Modification: Relevance to Adhesion, K.L. Mittal, ed., p. 363-378, VSP, May 1996).

The morphology of a polyimide film surface is modified from a semicrystalline state to an amorphous state without altering the bulk properties. The outer layer (0.5-25 nm) of fully cured poly(pyromellitic anhydride-oxydianiline) (PMDA-ODA) and poly(biphenyl dianhydride-p-phenylene diamine) (BPDA-PDA) polyimides is chemically modified to polyamic acid, which is subsequently imidized at 230-250°C for 30 min to give a disordered polyimide surface. This disordered layer seems amorphous since it swells well in 1-methyl-2-pyrrolidinone (NMP) and the ions in the modified layer can be easily removed with a solvent such as water or ethanol. The modified surfaces are analyzed by surface-sensitive techniques such as contact angle measurement, X-ray photoelectron spectroscopy (XPS), ion scattering spectroscopy (ISS), secondary ion mass spectroscopy (SIMS), and external reflectance infrared spectroscopy (ERIR). The adhesion of polyimide layers onto the amorphous polyimides is greatly enhanced. Interdiffusion and subsequent mechanical interlocking are the major contributors to the polyimide-polyimide adhesion. The relationship between the depth of modification and the peel strength is studied. The deeper the modification depth, the greater is the peel strength.

2389. Gribbin, J.D., L. Bother, and P. Dinter, “Process for passing a hydrophobic substrate through a corona discharge zone and simultaneously introducing an adhesive promoting aerosol,” U.S. Patent 5271970, Dec 1993.

A polymeric sheet structure consists of an adhesion-promoting coating on at least one surface of the substrate. The adhesion-improving coating is produced by treating this substrate surface with an electrical corona discharge between high voltage electrodes and a grounded counter-electrode while simultaneously spraying an aerosol into the corona discharge zone. The aerosol contains, for example, an aqueous emulsion of thermoplastic and/or crosslinkable components as an adhesion-promoting agent.

2144. Hozbor, M., “Plasma processes boost bondability of rubber and metal,” Adhesives Age, (Dec 1993).

29. Blitshteyn, M., and R. Wetterman, “Testing for surface energy,” Converting, 11, 44-46, (Dec 1993).

1679. Roth, J.R., L.C. Wadsworth, P.D. Spence, P.P.-Y. Tsai, and C. Liu, “One atmosphere glow discharge plasma for surface treatment of nonwovens,” in Proceedings of the 3rd Annual TANDEC Conference on Meltblowing and Spunbonding Technology, TANDEC, Nov 1993.

1293. Neagu, E, and R. Neagu, “Polymer surface treatment for improvement of metal-polymer adhesion,” Applied Surface Science, 72, 231-234, (Nov 1993).

The interaction between a low-pressure gas plasma and organic materials has mechanical (surface cleaning and dry micro-etching) and electrostatic (cross-linking and surface activation) effects. Corrosion of a fluorinated ethylenepropylene (FEP) sample was studied for different conditions. The corrosion rate of FEP depends on the gas and on the gas pressure and has the highest value for oxygen. The modifications of the sample surface were studied by contact-angle measurements for water and formamide and by the thermally stimulated discharge current method. The optimum parameters for a continuum vacuum metallization process of FEP are presented.

948. Podhajny, R.M., “Converters consultant: Is there a new trend toward using primers on films rather than corona treatment?,” Converting, 11, 16, (Nov 1993).

1953. Cueff, R., G. Baud, J.P. Besse, M. Jacquet, and M. Benmalek, “Surface free energy modification of PET by plasma treatment - influence on adhesion,” J. Adhesion, 42, 249-254, (Oct 1993).

Different cold plasmas have been used to treat the surface of polyethylene terephtalate (PET) in order to improve the adhesion of alumina thin films deposited by RF sputtering. The influence of these treatments on the surface free energy of the polymer is shown by a study of wettability. ESCA analysis of the PET surface suggests that chemical changes occur as the polymer is plasma treated.

The adhesion of alumina films on PET is studied by using tensile testing. The results show that the surface treatment of the PET by a slightly oxidizing plasma, such as carbon dioxide, increases by a factor of 1.7 the adhesion of alumina coatings.

1952. Carre, A., and J. Vial, “Simple methods for the prediction of surface free energy and its components: Application to polymers,” J. Adhesion, 42, 265-276, (Oct 1993).

The surface free energy of a polymer can be easily calculated by the Group Contribution Method developed by the authors. After having briefly recalled the method and illustrated it with new examples, the latest developments including the Weighted Group Contribution Method and the study of the molecular weight dependence of surface free energy are also expounded.

Finally, very simple means to determine the dispersive contribution to the surface energy are described. The dispersive component values calculated from the Lifshitz theory, and from the solubility parameters, are in good agreement with those obtained from wettability measurements.

204. Kutsch, W.P., “Hot stamping applications and critical surface tension in the plastic industry,” in SPE Decorating Div. RETEC 1993, Society of Plastics Engineers, Oct 1993.

1392. Markgraf, M.P., “Corona treatment: An adhesion promoter for UV/EB converting,” RadTech Report, 7, (Sep 1993).

2918. Sherman, P.B., “Corona discharge treatment,” in Conference Record of the 1993 IEEE Industry Applications Conference, 1669-1685, IEEE, Aug 1993.

Various aspects of corona discharge treatment are reviewed. Particular attention is given to the Lissajous power measurement procedure; the significance of quartz, ceramic, or rubber as the dielectric in corona treaters; watt density considerations; and stabilizers and fatty acids.

2754. Kuusipalo, J., and A. Savolainen, “Adhesion in extrusion coating with polypropylene,” in 1993 Polymers, Coatings and Laminations Conference Proceedings, 469-478, TAPPI Press, Aug 1993.

2282. Lander, L.M., L.M. Siewierski, W.J. Brittain, and E.A. Vogler, “A systematic comparison of contact angle methods,” Langmuir, 9, 2237-2239, (Aug 1993).

1954. Kloubek, J., and H.P. Schreiber, “Futher comments on contact angle measurements on polymer solids,” J. Adhesion, 42, 87-90, (Aug 1993).

In recent years much emphasis has been placed on the importance of specific interactions in determining a wide range of polymer properties. Following the work of Fowkes and coworkers,1,2 all non-dispersion force interactions falling into the “specific” category may be considered to arise from acid/base interactions. This places heavy emphasis on methods for determining suitable acid/base parameters for polymers, with inverse gas chromatography (IGC) as a convenient choice. The IGC approach employed by one of us3 uses Gutmann's theory4 of (Lewis) acids and bases, and determines polymer interaction properties by placing these in contact with vapors of selected fluids for which acidlbase indexes, AN and DN, are available. Retention volume data for interacting vapor/polymer combinations are compared with the retention volumes of dispersion-force probes (e.g., n-alkanes), leading to the identification of AN and DN parameters for the polymer.3

577. Silverstein, M.S., and Y. Sodovsky, “Wetting and adhesion in UHMWPE films and fibers,” Polymer Preprints, 34, 308-309, (Aug 1993).

539. Nicastro, L.C., R.W. Keown. J.S. Paik, and A.B. Metzner, “Effect of storage temperature on the heat sealability of polypropylene film,” TAPPI J., 76, 175-178, (Aug 1993).

537. Morita, M., N. Tsurata, and K. Morita, “Activation of wood surface by corona treatment to improve adhesive bonding,” J. Applied Polymer Science, 49, 1251-1258, (Aug 1993).

Oxidative activation of resinous wood surfaces by a corona treatment to improve adhesive bonding was studied. It was found that the wettability of the veneers, including hardwoods, softwoods, and tropical woods increased with an increase in the degree of treatment, and the gluability increased rapidly after the initial mild treatment. To elucidate the nature of any chemical change occurring on the wood surface, the dyeing examination of the wood and its components with Schiff's reagent was made, and the results showed a higher dyeing ability for corona-treated samples compared to untreated ones, indicating that aldehyde groups increased by the corona treatment. The treatment affected the alcohol-benzene extractives, and oxidized them to produce aldehyde groups. Especially, the neutral fraction in the extractives was significantly affected. On the other hand, negligible chemical effects of the treatment on the surface modification of the wood's main components were seen. Both the untreated and corona-treated samples adsorbed basic dye to the same extent of coloration. Thus, no measurable carboxyl groups increased on the surface of the samples. It seems that an increase in the wettability of corona-treated wood veneers resulted mainly from the oxidation of the high hydrophobic surface layer of neutral fraction substances in the extractives, and from the reduction in their hydrophobicity. © 1993 John Wiley & Sons, Inc.
https://onlinelibrary.wiley.com/doi/abs/10.1002/app.1993.070490714

358. Su, C.C., “Low volatile organic compounds coatings; surface energy considerations,” in 1993 Polymers, Laminations and Coatings Conference Proceedings, 491-499, TAPPI Press, Aug 1993.

299. Potts, M.W., M.H. Hansen, B.T. Kuettel, and J.D. Goins, “Effect of corona and flame treatments on extrusion coating performance properties,” in 1993 Polymers, Laminations and Coatings Conference Proceedings, 443-449, TAPPI Press, Aug 1993.

148. Gunnerson, R., “An aura of power,” Package Printing, 40, 24+, (Aug 1993).

82. DiGiacomo, J.D., “Advanced technology flame plasma surface treating systems,” in 1993 Polymers, Laminations and Coatings Conference Proceedings, 227-233, TAPPI Press, Aug 1993 (also in 36th Annual Technical Conference Proceedings, p. 356-361, Society of Vacuum Coaters, Nov. 1993).

56. Cheatham, C.M., J.L. Cooper, and M.H. Hansen, “Surface characterization of LDPE extrusion coatings after flame and corona treatments,” in 1993 Polymers, Laminations and Coatings Conference Proceedings, 321-328, TAPPI Press, Aug 1993.

852. Vargo, T.G., J.A. Gardella Jr., R.L. Schmitt, K.J. Hook, et al, “Low energy ion scattering spectrometry of polymer surface composition and structure,” in Surface Characterization of Advanced Polymers, Sabbatini, L., and P.G. Zambonin, eds., 163-180, VCH, Jul 1993.

851. Reed, N.M., and J.C. Vickerman, “The application of static secondary ion mass spectrometry (SIMS) to the surface analysis of polymer materials,” in Surface Characterization of Advanced Polymers, Sabbatini, L., and P.G. Zambonin, eds., 83-162, VCH, Jul 1993.

630. Desimoni, E., and P.G. Zambonin, “Spectroscopies for surface characterization,” in Surface Characterization of Advanced Polymers, Sabbatini, L., and P.G. Zambonin, eds., 1-5, Wiley-VCH, Jul 1993.

 

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