We have previously reported that the cuprous ion concentration inside the via increases during the reverse portion of a periodic reverse pulse waveform. The void decreases and bottom-up via filling is achieved by increasing this reverse current during copper electrodeposition. Acceleration occurs at the via bottom by increasing the reverse current for cathodic polarization. J. R. White's work showed a low cuprous ion concentration during cathodic polarization without additives. During cathodic polarization, the current density is high for copper dissolution and nitrogen gas bubbling with bis-(3-sulfopropyl) disulfide (SPS) and chloride, using the through-mask electrode trench. We have measured the increases in cuprous ion production with SPS and chloride additives using a rotating ring disk electrode. Copper electrodeposition is accelerated with SPS and chloride. An acceleration complex forms, which is based on the cuprous ion; i.e., Cu(I)-thiolate, a high cuprous ion concentration is observed at the through-mask electrode trench bottom. From a mass transfer study, therefore, the Cu(I)-thiolate complex accumulates in the through-mask electrode trench bottom. The current density increases at the through-mask electrode trench bottom and bottom-up filling then occurs.
We have already reported the cuprous ion concentration inside the via is closely related to void decreases and bottom-up via filling during copper electrodeposition. And further, observed the deposition current acceleration at through mask trench electrode when the substrate is pre-dissolved under nitrogen gas atmosphere with SPS and chloride added bath. In this paper we measured the changes in reaction intermediates concentration with the additives of SPS and chloride ion by using rotating ring disk electrode, and found as follows. In copper deposition at the disk electrode with adding Chloride and SPS or MPS, a marked increase in ring currents, which are the amounts of cuprous intermediates, were observed, and the largest current with 6ppm of MPS and 50ppm of Chloride. While, the ring deposition current markedly increased if the cuprous was supplied with additives of SPS and Chloride. MPS accelerate current more than SPS with cuprous supply.
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