A compression test for adhesion evaluation of diamond coatings

A key requirement of an effective coating is its adequate adhesion to the substrate. Thus, reliable test methods to evaluate coating adhesion and to characterize the deposition parameters affecting it are necessary for the systematic development of such coatings. The conventional technique for measuring diamond coating adhesion, the scratch test, is unreliable because of wear of the stylus and influences of the substrate. Thus, a noncontact technique (compression test) of evaluating the adhesion of diamond coatings on brittle substrates was modelled and developed. This method utilizes the differences in Young's modulus between the coating and the substrate via application of an external load in order to generate interfacial stresses and debond the coating. An innovative three-dimensional numerical model, based on combining the variational and boundary integral approaches, was utilized to link the indirect (i.e. load) to the direct (i.e. debond shear stress or elastic energy of delamination) characteristics of adhesion. Factors affecting the adhesion strength of the diamond coatings are discussed in relation to the process parameters. This test offers an excellent alternative to conventional techniques for measuring the adhesion strength of diamond coatings on brittle substrates.     

Adhesion properties and fracture mechanism of plasma sprayed NiCrAl/Al2O3–13wt.%TiO2 coatings by post annealing

Plasma-sprayed NiCrAl/Al₂O₃–13wt.%TiO₂ coatings (AT13) deposited on mild steel substrate were annealed with varying temperatures in air. The adhesion of the coating was evaluated by tensile adhesive strength test. The microstructure and the fracture mechanism were studied using optical microscopy, X-ray diffraction, and scanning electron spectroscopy/energy dispersive spectroscopy. It was found that the tensile bond strength of the coatings increased with increasing of annealing temperature at first and then decreased with increasing of annealing temperature further. The as-sprayed coating fractured at the interfaces of substrate/bond layer and bond layer/ceramic coating with a brittle–ductile mixed fracture. The measured strength expressed the adhesive strength and internal adhesive strength of the coating. The failure of the coating annealed at 300, 400, and 500 °C took place at the interface of substrate/bond layer and had a mixed fracture surface of transgranular cleavage fracture and localized ductile fracture. The strength obtained is the adhesive strength between the coating and the steel substrate. The coating annealed at 400 °C had a maximum strength of 42.9 MPa. When the temperature is above 600 °C, the bonding strength would be damaged. Therefore, there is a proper annealing temperature which can significantly improve the bond strength of the coating.     

Elastica bend testing of the effective interfacial shear strength and critical deformation strains of brittle coatings on ductile substrates

An elastica bend test is described that provides a rapid, convenient, and reproducible means for examining the interfacial delamination of brittle coatings on ductile substrates. By bending a coated strip into a half-loop and examining the microscopic cracking that is observed on the sample surface as the loop size decreases, information is obtained about the characteristic initial, mean, and final strains _i, _m and _f that describe the distribution in strength of the coating. By measuring the distance between the cracks at high strains, we obtain an estimate of the interfacial shear strength τ.     

Internal stresses and adhesion of thin silicon oxide coatings on poly(ethylene terephthalate)

The effect of internal stresses on the cohesion and adhesion of a thin silicon oxide (SiO_x) oxygen-barrier coating, evaporated on a poly(ethylene terephthalate) (PET) film substrate was studied. Internal stresses were generated during annealing in the temperature range for recrystallization of the PET,during calendering in a multilayer structure where two SiO_x /PET films were laminated together with a polypropylene film, and during long-term thermal aging below the glass transition temperature of the polymer. The cohesion of the coating and its adhesion to the polymer substrate were derived from fragmentation tests, in which the failure of the oxide coating was analyzed as a function of the applied stress during uniaxial tensile loading of the substrate. The intrinsic coating strength at critical length and the interfacial shear strength were found to be equal to 1350 MPa and 73 MPa, respectively. It was found that none of the thermal treatments investigated altered the interfacial interactions. Rather, these treatments induced shrinkage of the PET substrate, which increased the coating internal compressive stress and the SiO_x /PET interfacial shear strength. A linear relationship between the SiO_x /PET interfacial shear strength and the coating internal stress was determined from a stress transfer analysis. The coefficient of this linear relationship, equal to-1.34 · h _c/l _c, where h _c is coating thickness and l _c is the critical stress transfer length, reproduces the experimental data with good accuracy.     

Evaluation of the weld-line strength of thermoplastics by compact tension test

In order to understand the relationship between processing conditions and the properties of weld-lines on a molecular level, it is necessary to evaluate the true strength of the weld-line that is not affected by the V-shape notch on the surface of the weld-line zone. In this experiment, the weld-line strength of several brittle, ductile, or phase-separated polymers was evaluated using the compact tension test by measuring the critical stress intensity factor, K_IC, or the critical J-value, J_IC, and the results were compared with those obtained by tensile testing. For brittle polymers such as poly(methyl methacrylate) (PMMA) or styrene acrylonitrile copolymer (SAN), the value of the weld-line factor, i.e., the strength ratio between the welded and the non-welded specimen, is higher than that measured by tensile testing, because of the notch sensitivity of brittle thermoplastics and the notch dependence of tensile strength. On the other hand, in the case of ductile polymers such as polycarbonate (PC), the weld-line factor is similar for both the tensile and compact tension tests. However, the dependency of the weld-line factor on melt temperature is more obvious in the compact tension test. From these results, it seems that the compact tension test is more appropriate for measuring the interfacial adhesion strength across the weld-line, which excludes the notch effect.     

Effect of inter-plies on the short beam shear delamination of steel/composite hybrid laminates

Interlaminar shear test methods (ILS) were implemented to characterize the delamination behavior of asymmetric steel/carbon fiber reinforced plastic (CFRP) hybrids. To improve the delamination behavior thermoplastic inter-plies were inserted between CFRP and steel. Supported by optical strain measurement the maximum shear stress (τ_MAX), the shear stress at interfacial delamination (τ_IF) and the shear stress at large-scale CFRP ply delamination τ_D were evaluated. The significant effect of inter-plies on the adhesion was best reflected by the shear stress value at interfacial delamination. Finite element analysis of the actual shear stress distribution in an asymmetric hybrid sample without inter-ply revealed that the calculated shear strength is just slightly overestimated compared to the standardized evaluation procedure.     

Role of Sn on the adhesion in Cu–Sn alloy-coated steel–rubber interface

Cu–Sn coatings with varying Sn content were deposited on steel substrate by immersion route and the effect of variation of Sn content and the substrate roughness on the interfacial adhesion strength of Cu–Sn-coated steel substrates vulcanized with styrene butadiene rubber were investigated. The surface roughness of the coatings did not vary compared to pristine steel substrate with change in Sn weight% in the coatings. The coated surfaces exhibited bare spots or deep trough as micro-discontinuities in the coatings, where formation of Fe₂O₃ was evident from SEM-EDS, AES, and XPS analysis. Microstructural study of the coating cross-section and coating-substrate interface by transmission electron microscopy of cross-sectioned samples revealed inadequate penetration of coating inside these troughs. Peel test carried out on the Cu–Sn-coated steel–rubber joints showed mixed mode i.e. adhesive and cohesive mode of interfacial fracture irrespective of the coating composition. The peel test further indicated higher interfacial adhesion strength for Cu–Sn-coated samples than pure Cu-coated samples, with an optimum adhesion strength for the coatings containing 3–4?wt.% Sn.     

The brittle‐ductile transition temperature of polycarbonate as a function of test speed

The fracture behavior of polycarbonate was studied as a function of temperature (?80°C to +80°C) and test speed (10^?5 to 10 m/s) using an instrumented, singleedged, notched tensile test (SENT). SENT tests give information on the fracture stress, fracture displacements, and fracture energies of polycarbonate, and from these data the average crack speeds were calculated and the brittle‐ductile transitions were determined. The fracture stress and the fracture energies of ductile fracturing samples increased with increasing test speed. The fracture surfaces were studied by scanning electron analysis, and sometimes a mixed mode fracture, part ductile and part brittle, could be seen. At high test speeds, a sharp brittle‐ductile transition was observed, while at low test speeds the transition was more gradual, via a mixed mode region. This mixed mode region decreased in size with increasing test speed and was absent at the higher test speeds. The average crack speeds in the ductile region were directly related to the test speeds. The brittle‐ductile transition temperature increased with the logarithmic of the test speed.     

The Interfacial Bond Strength in Glass Fibre-Polyester Resin Composite Systems

The interfacial bond strength in glass fibre-polyester resin composites has been investigated using various experimental techniques. These included blocks of resin containing fibre (in which, depending on the geometry of the specimen, failure occurs in either a shear or tensile mode) the pullout of a fibre from a disc of resin and a short beam shear test for interlaminar shear strength determination.

Low power optical microscopy and optical retardation measurements of stress induced birefringence were used to detect the difference between intact and debonded fibre resin interfaces. The shear modulus and shear strength of the resin were obtained from torsion tests on cylindrical rods of the resin.

The single fibre shear debonding specimen and the short beam shear test are shown to be the most viable test methods but interpretation of the results is complicated by the various modes of failure possible and by the different stress states which exist in the area of the specimen where debonding starts. Stress concentration factors obtained by finite element analysis and photoelastic analysis have been applied to the results from these tests and the corrected interfacial bond strengths are in close agreement.

The real interfacial bond strengths of well bonded glass-fibre polyester resin systems is shown to be of the order of 70 MN m^?2.     

Effect of surface treatments on interfacial adhesion energy between UV-curable resist and glass wafer

The interfacial adhesion energy between the resist and the substrate is very important in nanoimprinting because of problems with the resist sticking or pulling off during separation of the mold from the substrate. Substrate surface treatments with a self-assembled monolayer or oxygen plasma provide good adhesion between a resist coating and a silica substrate. In this paper, we describe the adhesion properties of a resist and a glass wafer measured using the four-point bending test. The interfacial adhesion energy between the resist and the glass wafer was evaluated for various substrate surface treatments of adhesion promoters and anti-sticking layers. The interfacial fracture energy without treatment was 1.23 J/m², and was in the range 0.49–2.57 J/m² for the other treatments tested. The interfacial fracture surfaces were also investigated by field emission scanning electron microscopy, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy to determine the fracture mode at the interfaces.     

Friction induced paint damage as affected by clearcoat chemistry

One form of damage to automotive painted plastic composites, in particular thermoplastic bumpers and fascias, is known to be caused from compressive shear loading placed on the surface of the composite. The loading inflicted upon the composite by a stationary force (e.g. an automobile hitting a post) or a moving object (e.g. an automobile hitting another automobile), and consequent compressive shear that is induced, can result in cohesive delamination of the substrate. The cohesive delamination in the painted composite (herein referred to as ‘gouge') is not only influenced by the cohesive strength of the substrate but also by the mechanical properties of the coating. Our studies indicate that one important attribute of the coating, namely the coating's coefficient of friction, can significantly impact the ‘gouge' resistance of the painted composite. In this work, we will describe the derivation of coating attributes as they affect ‘gouge' resistance and relate changes in the coating chemistry to useful life parameters.     

Fracture behavior of diamond-like carbon films on stainless steel under a micro-tensile test condition

We investigated the stability of the DLC film coated on 304 stainless steel substrate by r.f. PACVD method. Fracture and spallation behaviors of the coating were observed during micro-tensile test of the film/substrate composite. As the tensile deformation proceeded, the cracks of the film appeared in the perpendicular direction to the tensile axis. Further deformation resulting in the local necking with shear band of 55° inclined to the tensile axis, induced the spallation of the film, which was initiated at the cracks of the film, and was aligned along the slip directions. We found that both the cracking and the spallation behaviors are strongly dependent on the pretreatment condition, such as Ar plasma pretreatment or Si buffer layer deposition. The spallation of the film was significantly suppressed in an optimized condition of the substrate cleaning by Ar glow discharge. These results show that the spallation behavior during the tensile test can be used to estimate the interfacial strength of the coating with relatively poor adhesion.     

The role of ion-induced substrate damage in thin film adhesion strength

Variable-energy positrons are combined with Auger electron spectroscopy, scanning electron microscopy, and scratch test critical load measurements to study interfacial properties in thin film adhesion. This work complements an earlier investigation of the adhesion strength enhancement produced by ion bombardment of the substrate surface before deposition. In this study, we have investigated SiO₂ films deposited by radio-frequency (RF) sputtering onto stainless steel substrates. Extended ion bombardment etching leads to three related effects: the scratch test critical load is increased significantly, Auger electron spectroscopy shows a greater penetration of the film material into the substrate; and the interfacial positron annihilation signal is dominated by large, open-volume defects. These results are interpreted as confirmation that ion bombardment leads to the formation of microvoids in the interface layer and, consequently, to an increased adhesion strength by allowing mechanical interlocking between the coating and the substrate.     

An energy-based failure criterion for delamination initiation in electronic packaging

The significance of interfacial delamination as a crucial failure mechanism in electronic packaging has been documented in many papers. A number of failure criteria have been used to solve the problems with a pre-crack at the interface. However, in real electronic packages, the size and location of the cracks or/and delamination cannot be predicted. It is not easy to use the traditional fracture criteria to deal with more complicated 3D delamination problems. The epoxy molding compound (EMC)/copper leadframe interface was selected in this study. A series of button shear tests were conducted to evaluate the interfacial adhesion between the EMC and copper. In each test, the failure load acting on the EMC of the button shear sample was measured at different shear angles and a finite element model was used to evaluate the stresses at the EMC/copper interface. In this paper, an energy-based failure criterion is proposed using both the interfacial distortional and hydrostatic strain energy densities as two failure parameters. Stresses were extracted from the numerical simulation in order to calculate the interfacial distortional strain energy density, U _d, and the interfacial hydrostatic strain energy density, U _h, related, respectively, to the shear and tensile modes. U _d and U _h were averaged within a selected region of the finite element model where it exhibits high interfacial strain energy density values.     

Strength of cylindrical butt joints bonded with epoxy adhesives under combined static or high-rate loading

The influence of loading rates and the combined stress states of tension and shearing on the strength, strain, and absorbed energy of an adhesively bonded joint was experimentally investigated. Cylindrical butt joint specimens were prepared and strength tests were performed on the specimens with a servo-controlled hydraulic testing machine that combined tension and torsion loading. Two types of epoxy adhesives, ductile and brittle, were applied to the specimens. The tests were performed under a quasi-static condition of 6.67×10⁻² MPa/s and a high-rate loading condition of 1.00×10³ MPa/s. The results of the combined loading tests showed that the states of the fractured surfaces were not affected by the loading rates. As for the ratio of tensile and shear loading, adhesive failure tended to partially occur when the ratio of shear loading was very high. The strength points for the specimens bonded with each adhesive were distributed in a stress plane of tension and shearing and could be fitted with a curve that was described by an equation with exponential parameters that were not influenced by the strain rate; however, other parameters that described the intercepts were influenced. The failure strains and absorbed energies for the brittle adhesive were slightly dependent on the strain rate, but this dependency was unclear for the ductile adhesive.     

拉伸法测定涂层界面强度的适用性研究

评述了用于测定涂层界面强度的几种主要测试方法的优点与不足，分析了拉伸法的适用条件与范围。指出拉伸法仅适于测定弹性模量大于金属基体的脆性薄涂,但测试值与界面结合强度的真实值有较大差异。当涂层的变形能力大于金属基体的变形能力时，该法无法测定涂层－金属基体界面结合强度。研究了不同固化工艺的胶粘剂粘涂层在拉伸法中的应变与拉伸载荷的关系，结果表明该法在粘涂层的形变能力较大时无法获得涂层开裂的信号。     

Influence of adding multiwalled carbon nanotubes on the adhesive strength of composite epoxy/sol–gel materials

The tensile shear strength of a composite epoxy/sol–gel system modified with different ratios of multiwall carbon nanotubes (MWCNTs) was evaluated using a mechanical testing machine. The experimental results showed that the shear strength increased when lower than ~0.07 wt% of MWCNTs were added in the composite solution. The increase of the shear strength was attributed to both the mechanical load transfer from the matrix to the MWCNTs and the high specific surface area of this material that increased the degree of crosslinking with other inorganic fillers in the formulation. However, a decrease in the adhesive shear strength was observed after more than ~0.07 wt% MWCNTs were added to the composite. The reason for this may be related to the high concentration of MWCNTs within the matrix leading to excessively high viscosity, dewetting of the substrate surfaces, and reduced bonding of MWCNTs with the matrix, thereby limiting the strength. SEM observation of the fracture surfaces for composite epoxy/sol–gel adhesive materials with 0.01 wt% MWCNTs showed a mixed interfacial/cohesive fracture mode. This fracture mode indicated strong links at the adhesive/substrate interface, and interaction between CNTs and the matrix was achieved; therefore, adhesion performance of the composite epoxy/sol–gel material to the substrate was improved. An increase of a strong peak related to the C–O bond at ~1733 cm^?1 in the FTIR spectra was observed. This peak represented crosslinking between the CNT surface and the organosilica nanoparticles in the MWCNTs-doped composite adhesive. Raman spectroscopy was also used to identify MWCNTs within the adhesive material. The Raman spectra exhibit peaks at ~1275 cm^?1 and in the range of ~1549–1590 cm^?1. The former is the graphite G-band, while the latter is the diamond D-band. The D-band and G-band represent the C–C single bond and C=C double bond in carbon nanotubes, respectively.     

Low density polyethylene-polypropylene blends: Part 1 - Ductility and tensile properties

Abstract

The composition-property relationships of LDPE-PP binary blends have been investigated. Young's modulus, yield strength and flexural strength of the blends varied monotonically with composition, whereas the elongation at failure and the true ultimate tensile strength for the blends with 30-50 wt-% PP exhibited synergetic effects. These blends showed strong cold draw hardening, and their elongations at failure and the true ultimate tensile strengths were much higher than those of the neat components. Meanwhile, impact strength showed an abrupt reduction with increasing PP content and the failure mode changed from ductile to brittle in the composition range of 30-50 wt-% PP. Failure mechanisms are discussed, addressing interfacial adhesion between LDPE and PP and the non-uniform shrinkage of the component domains upon cooling.     

The use of a modified microindentation technique to evaluate enviro-mechanical changes in composite interphase properties

Fiber sizing can improve the performance of fiber-reinforced polymer composites. The focus of this work was to determine if the improvement in performance could be ascertained from a micromechanical test for interfacial adhesion on as-processed materials under hygrothermal exposure. Three types of sizings were examined: a carboxyl modified poly(hydroxyether), that is identified as low spread phenoxy (LSP), a poly(vinylpyrrolidone) (PVP) sample and a standard industrial sizing (G′). A nanoindenter was effectively used to obtain interfacial shear strength (IFSS) using a modified micro-indentation technique. The results showed that LSP outperforms the PVP and G′ materials in bulk composite properties, but showed equivalent interfacial shear strength to G′ and experienced hygrothermal degradation in interfacial adhesion that the PVP did not. The LSP composite loses 10% of its original interfacial shear strength after 576 h, while for PVP composite it improves by 25%. The tensile strengths for LSP and PVP composites decrease by 7% and 10%, respectively, at 576 h of hygrothermal exposure. The relationship between tensile strength and interfacial adhesion proved to be weak, but processing defects and other failure processes showed a strong influence of interfacial adhesion on tensile strength of compsites.     

Plasma etching and plasma polymerization coating of carbon fibers. Part 1. Interfacial adhesion study

Unsized AS-4 carbon fibers were etched by RF plasma and then coated via plasma polymerization in order to enhance their adhesion to vinyl ester resin. Gases utilized for plasma etching were Ar, N₂ and O₂, while monomers used in plasma polymerization coating were acetylene, butadiene and acrylonitrile. Plasma etchings were carried out as a function of plasma power (30–70 W), treatment time (1–10 min) and gas pressure (20–40 mtorr). Plasma polymerizations were performed by varying the treatment time (15–60 s), plasma power (10–30 W) and gas pressure (20-40 mtorr). The conditions for plasma etching and plasma polymerization were optimized by measuring interfacial adhesion with vinyl ester resin via micro-droplet tests. Plasma etched and plasma polymer coated carbon fibers were characterized by SEM, XPS, FT-IR and α-Step, dynamic contact angle analyzer (DCA) and tensile strength measurements. In Part 1, interfacial adhesion of plasma etched and plasma polymer coated carbon fibers to vinyl ester resin is reported, while characterization results including tensile strength of carbon fibers are reported in Part 2. Among the treatment conditions, a combination of Ar plasma etching and acetylene plasma polymer coating provided greatly improved interfacial shear strength (IFSS) of 69 MPa, compared to 43 MPa obtained from as-received carbon fiber. Based on the SEM analysis of failure surfaces and load-displacement curves, the failure was found to occur at the interface between plasma polymer coating and vinyl ester resin.