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Four-point bend fracture mechanics are then used to quantify the interfacial adhesion energy of the Cu/TaN interface, Table 3.1. The copper SFD reaction temperature is between 270 – 285 oC for all depositions. Precursor concentration is between 0.2 – 0.9 wt. % and hydrogen concentration is approximately 0.5 wt. % for all depositions. The hydrogen concentration is always in excess of 100 times the necessary amount needed for complete conversion of the loaded Cu(tmod)2. X-ray photoelectron spectroscopy (XPS) is used to confirm crack propagation at the interface of interest. Table 3.1: Table of adhesion energy for untreated and poly(acrylic acid) treated samples. Sample group Cu thickness (nm) Cu/TaN adhesion energy (J/m2) Variation (J/m2) Untreated A-1 68 0.55 0.25 A-2 97 1.40 0.37 A-3 126 0.56 0.05 A-4 131 1.56 0.20 A-5 180 0.50 0.03 Treated B-1 130 >5.3* N/A B-2 172 3.36 0.57 B-3 190 4.69 0.20 B-4 192 >5.3* N/A B-5 266 5.32 0.92 * Pre-crack failed to grow into interface Untreated sample stacks have a copper thickness range of 68 – 180 nm. PAA pretreated stacks have a copper thickness range of 130 – 266 nm. It is observed that the growth rate of copper is faster on PAA pretreated samples as compared to samples that did not have a pretreatment for equivalent reaction conditions. A typical load versus displacement curve for an untreated and PAA pretreated stack is shown in Figure 6 and Figure 7, respectively. The steady state load is determined 66PDF Image | Supercritical Fluid Deposition Of Thin Metal Films
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