This work examines the mechanical performance of thin film coatings from Photosensitive-benzocyclobutene (Photo-BCB) formulations (Cyclotene2 4024, 4026 and 7200), on various substrate surfaces such as Al, Cu, Si, and SiN. The adhesion promoter used was designated AP-3000 and was based on vinyltriacetoxysilane (VTAS), which had been properly hydrolyzed and advanced. Measurement of the interfacial adhesion was performed primarily using the modified Edge Liftoff Test m-ELT. It was found that, by applying the newly developed adhesion promoter, AP-3000, the interfacial energy of Photo-BCB to Al, Cu, Si, and SiN was significantly improved, often approaching the toughness of Photo-BCB, ca. 45 J/m2. The x-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) analyses of the delaminated surfaces of the Photo-BCB/Al structure revealed distinct differences in surface roughness and the chemical composition depending on whether or not adhesion promoter was used. Other parameters important for long term stability (e.g., moisture uptake and thermal stability) of Photo-BCB were also measured. The equilibrium moisture content at 84 percent RH in ambient temperature was low, 0.14 wt percent and the thermally induced weight loss at 330°C in helium atmosphere was less than 1 percent/h. The low moisture absorption and good thermal stability, together with the given mechanical toughness and adhesion, allow the Photo-BCB to be widely usable for various microelectronic packaging applications, for up to 40 μm thick build in the case of silicon substrate. [S1043-7398(00)00701-5]
The thermal polymerization reaction of divinyl siloxane bis-benzocyclobutene (DVS bis-BCB) was monitored in-situ with FT-IR spectroscopy in order to follow specific chemical changes and determine the reaction order and rate constants at temperatures from 150° to 210°C. FT-IR spectra were obtained at regular intervals throughout the reaction with a Nicolet 170SX spectrophotometer.Monomeric DVS bis-BCB contains mixed stereo and positional isomers of 1,3- bis(2-bicyclo[4.2.0]octa-1, 3, 5-trien-3-ylethenyl)-1, 1, 3, 3-tetramethyl disiloxane (CAS 117732-87-3). It polymerizes via Diels-Alder cycloaddition reactions between vinyl groups and an intermediate o-quinodimethane formed by first-order, thermally initiated ring openings of the benzocyclobutene rings. Gaseous byproducts are not produced; therefore, the cure is easier to manage than are cures for polyimides which evolve water in polycondensation reactions. The DVS bis-BCB has four reactive elements per monomer unit and, thus, polymerizes into a very highly cross linked and solvent resistant network.With the FT-IR methodology, the reaction was easily monitored through the points of gel formation and vitrification. With the exception of DSC (i.e., calorimetry) which does not sense specific chemistry, other methods were not successful in following the reaction after a gel was formed. We have found that the polymerization was first-order until vitrification occurs; the gelation alone had no apparent effect on the reaction rate.DVS bis-BCB is under development at Dow as high performance dielectric material for multilayer interconnect coating applications for the microelectronics industry. Methodology reported here is employed in developing effective cure management strategies.
The concentration dependence of the conformational dynamics of polymer solutions as revealed by measurements of oscillatory flow birefringence (0.f.b.) has been obtained for narrow-distribution linear, comb and regular-star molecules for concentrations in the range c[q] 5 11. The data obtained show that the relaxation-time spectrum is affected markedly by
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