Surface Properties and Adhesion of Flame Treated Sheet Molded Composite (SMC)

The surface chemistry of sheet molded composite (SMC) following interaction with a natural gas/air flame operated under reducing, stoichiometric, and oxidizing conditions has been investigated. The SMC surface chemistry is altered to contain in addition to hydrocarbon, ether, and ester functional groups, carbonyl and a greater carboxyl concentration. The extent of surface oxidation varies with the flame condition in the manner oxidizing ～ stoichiometric > reducing. Lap shear tests carried out at 82°C (180°F) for coupons bonded with a urethane adhesive did not fail by fiber tear. Surface analysis results indicate failure at an oxidized SMC-adhesive/non-oxidized SMC interface and within the non-oxidized SMC surface.     

An Investigation of the Effect of Plasma Treatment on the Surface Properties and Adhesion in Sheet Molded Composite (SMC) Material

Sheet molded composite was treated with different plasmas (oxygen, dry air, nitrogen, and argon). Plasma treatment of SMC alters the surface properties in a manner dependent on the type of plasma used and the time of treatment. The surface properties were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Fourier transform infrared spectros-copy (FTIR). A two-part urethane adhesive was used to prepare lap shear specimens. Untreated SMC, plasma-treated SMC, and primer-treated SMC were prepared, bonded and tested. The surface properties of the failed specimens were measured. The adhesion characteristics of SMC and the surface properties of the failed specimens were correlated with the type of treatment and the surface properties of treated SMC. Comparison of the surface and adhesive properties of plasma-treated samples with those for untreated samples indicates a) an increase in roughness, b) an increase in the level of SMC surface oxidation, and c) an increase in the failure force for lap shear tests.     

An Investigation of the Effect of Plasma Treatment on the Surface Properties and Adhesion in Sheet Molded Composite (SMC) Material

Sheet molded composite was treated with different plasmas (oxygen, dry air, nitrogen, and argon). Plasma treatment of SMC alters the surface properties in a manner dependent on the type of plasma used and the time of treatment. The surface properties were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Fourier transform infrared spectros-copy (FTIR). A two-part urethane adhesive was used to prepare lap shear specimens. Untreated SMC, plasma-treated SMC, and primer-treated SMC were prepared, bonded and tested. The surface properties of the failed specimens were measured. The adhesion characteristics of SMC and the surface properties of the failed specimens were correlated with the type of treatment and the surface properties of treated SMC. Comparison of the surface and adhesive properties of plasma-treated samples with those for untreated samples indicates a) an increase in roughness, b) an increase in the level of SMC surface oxidation, and c) an increase in the failure force for lap shear tests.     

The Effect of Surface Preparation and Exposure Environment on the Bond Failure Processes in Adhesively Bonded Sheet Molded Composite (SMC)

The durability of adhesively-bonded composites has been investigated using a wedge-type specimen. Polyester-resin, fiberglass sheet molded composite (SMC) was bonded with a commercial two-part poly-urethane adhesive. The SMC composite received one of four different surface preparations: no treatment, abrasion, priming, or abrasion and priming. The wedge test was used to study the durability of the samples which were exposed to air and to the vapor above water, concentrated ammonium hydroxide, or methanol at 60[ddot]C. The crack length was measured during the experiments. The crack growth rate as a function of surface treatment varied in the manner: untreated ≈ abraded > primed ≈ abraded and primed. The crack growth rate as a function of vapor changed in the manner: methanol > ammonium hydroxide > water ≈ air. The samples were removed at the conclusion of the test and the failure mode was determined visually, by scanning electron microscopy (SEM), and by X-ray photoelectron spectros-copy (XPS). Initial insertion of the wedge resulted in substrate failure (delamination of the composite). Exposure of untreated and abraded samples under stress to the test vapors promoted adhesive failure. Primed and abraded/primed samples under stress and exposed to methanol vapor debonded via cohesive processes.     

Characterization of Surface Pretreatments on Al/Li Alloy and Related Mechanical Properties of Polysulfone Adhesive Bonds

An investigation of polysulfone-Al/Li alloy interaction involved single lap shear joints and wedge samples following an FPL etch, sulfuric acid anodization (SAA) and phosphoric acid anodization (PAA). The study of the Al/Li surfaces involved the determination of the elemental composition and morphological features of the pretreated adherend before bonding and following fracture. When polysulfone was either thermally pressed or primed onto the microporous surface, the polysulfone indeed penetrated into the porous oxide and thereby provided a mechanical means of adhesion. The wedge test results for the adherend pretreated by PAA and SAA were superior to those for the FPL etched adherend. The failure path for the FPL etched samples was at the adhesive/oxide interface whereas the failure path for the PAA samples was within the adhesive but with occasional divergence of the crack into the oxide. The porous oxides on Al/Li alloy formed after PAA and SAA treatment were shown to undergo dramatic changes in morphology on short term (< 95 hrs) exposure to 71°C and 100% R.H. environment. The mechanism of failure was due to moisture which caused hydration and subsequent weakening of the surface oxide layer and the bonded joint. Lithium was not surface concentrated in the PAA treated Al/Li alloy as shown by AES depth profiling and therefore the effect of Li on the durability of the bonded alloy is considered minimal.     

Surface Chemical Characterization of Copper Oxide and its Relationship to Adhesion in Formed Epoxy/Copper Interfaces

Experiments have been performed to comprehensively analyze copper oxides formed from a chlorite oxidation bath on copper bar stock and to measure the adhesion of an epoxy casting resin to the corresponding oxidized surfaces. Temperature conditions for the bath ranged from 25 to 90°C with oxidation times between 0.25 and 20 minutes. Adhesion testing of the epoxy/copper systems was performed using a 3-point bend testing rig and measuring the ultimate force and displacement at the moment of sample failure near the epoxy/substrate interface. The flexure testing configuration used the resin as a stiffening rib which created a deviation in the force-deflection curve from that of the originally-oxidized copper bar stock. As the oxidation temperature increased above 50°C, there was higher cohesion of the oxide layer formed on the copper and that led to a higher measured force at failure. On copper samples oxidized at lower temperatures, failure occurs within the oxide as a part of the latter remains on the resin side and lower adhesion was measured.     

Relaxation Properties and Chemical Nature of Polymer Surface Layers as Related to the Strength of Adhesive Joints with Metals

A new approach based on the theory of elasticity is proposed to study relaxation properties of adhesive transition layers. It involves experimental evaluation of the rate dependence of the fracture energy of the bulk polymer and its adhesive joint.

The investigation of the interaction of a polymer surface layer with electroplated copper by XPS using the effect of differential charging (the latter produced by potential shift of the sample by 10V), makes it possible to identify the functional groups of adhesive brought into contact with substrate surface. For ABS copolymers a bond of -O … Cu type was formed.

The mechanism of adhesive contact formation and factors affecting the strength of adhesive joints could be understood better by determining the properties of surface and transition layers.     

Surface structures of solvent‐cast films prepared from poly(ethylene oxide)‐segmented nylons

The surface structures of three kinds of poly(ethylene oxide)‐segmented nylon (PEO‐Ny) films prepared by the solvent‐cast method were investigated with electron spectroscopy for chemical analysis (ESCA). The PEO‐Ny's used were high‐crystalline PEO‐segmented poly(iminosebacoyliminohexamethylene), low‐crystalline PEO‐segmented poly(iminosebacoylimino‐m‐xylene), and amorphous PEO‐segmented poly(iminoisophthaloyliminomethylene‐1,3‐cyclohexylenemethylene), and the PEO contents in the bulk polymers were approximately 10 wt %. The ESCA results showed that the PEO segment was enriched on the top surfaces of all the films, and the degrees of enrichment were different. The mechanism of the PEO enrichment was examined. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 10–16, 2002     

表面原位化学组合改性Al（OH）3粉体的机理研究

采用表面原位化学组合的方法，在Al（OH）3表面分批结合上甲苯二异氰酸酯（TDI）、烷基酚醛树脂（PF）、丁腈橡胶（NBR）等几种改性剂，形成极性逐渐过渡的梯度界面层。电镜分析表明，Al（OH）3颗粒的平均粒径随改性剂种类的增加依次减小。通过红外光谱、热分析证明了改性剂在Al（OH）3的表面原位形成多层化学键合结构，得到“硬核-软壳”结构的粒子，从而提出表面原位化学组合改性Al（OH）3粉体的微观相界面模型，解释了表面原位化学组合方法改性Al（OH）3填充PVC复合材料具有良好力学性能的原因。     

Chemical Composition and Surface Properties of Paper Mill Sludge and their Impact on High Density Polyethylene (HDPE) Composites

A comparative study was conducted using paper mill sludge from three different pulping processes at two primary sludge (PS) to secondary sludge (SS) ratios to better understand the role of PS and SS in the development of wood/high-density polyethylene (HDPE) composite properties. Sludge samples from a thermomechanical (TMP), chemico-thermomechanical (CTMP), and Kraft pulping process were used at three proportions (20, 30, and 40%) to produce different composites. Pulp and combined sludge samples were characterized by conventional chemical analysis and FTIR spectroscopy. FTIR spectroscopy enabled the characterization of the inorganic content in the sludge. Results showed that the variation in composite properties according to sludge type could be explained by the chemical composition, regardless of pulping process or SS:PS ratio. Ash and cellulose content were the dominant factors in explaining the composite mechanical properties, and nitrogen content, although low, was the dominant factor in explaining composite toughness.     

Surface chemical analysis of poly(ε‐caprolactone)–perfluoropolyether–poly(ε‐caprolactone) triblock copolymers by X‐ray photoelectron spectroscopy

The air‐side surface composition of a series of poly(ε‐caprolactone)–perfluoropolyether–poly(ε‐caprolactone) triblock copolymers with different compositions and block lengths have been studied by angle‐dependent X‐ray photoelectron spectroscopy (XPS). The weight percentage of the perfluoropolyether (PFPE) and polycaprolactone (PCL) blocks, and ethylene oxide linker (R_H) has been calculated in different ways: from C1s, O1s and F1s photoemission peaks and by line fitting of the C1s and O1s envelopes. The atomic sensitivity factors and the parameters used to fit the peak envelopes have been experimentally determined using some reference materials. A critical discussion of the different methods used in the surface characterization and the degradation of PFPE segments, induced by irradiation beam, have been also reported. A large excess of PFPE with respect to the bulk composition was observed in all samples, and the angular dependence of the XPS signal demonstrated that the content of the fluorinated block segment increased by decreasing the sampling depth. The PFPE surface concentration was also decreased by increasing the PCL/PFPE ratio, but the surfaces of the samples were still dominated by PFPE segments for copolymers with a bulk PFPE composition lower than 10%. Moreover, copolymers with similar PCL/PFPE bulk ratios but with different PFPE block lengths, showed similar PFPE surface composition when the number‐average molecular weight (M_n) was 2000 and 3200 g mol^?1, while that observed for copolymers containing PFPE block with M_n 900 g mol^?1 was lower. Copyright © 2003 Society of Chemical Industry