Provided herein are methods of depositing void-free cobalt into features with high aspect ratios. Methods involve (a) partially filling a feature with cobalt, (b) exposing the feature to a plasma generated from nitrogen-containing gas to selectively inhibit cobalt nucleation on surfaces near or at the top of the feature, optionally repeating (a) and (b), and depositing bulk cobalt into the feature by chemical vapor deposition. Methods may also involve exposing a feature including a barrier layer to a plasma generated from nitrogen-containing gas to selectively inhibit cobalt nucleation. The methods may be performed at low temperatures less than about 400° C. using cobalt-containing precursors.

Method for void-free cobalt gap fill

https://iopscience.iop.org/article/10.1149/2.0111709jss/pdf

Citric Acid as a Complexing Agent in Chemical Mechanical Polishing Slurries for Cobalt Films for Interconnect Applications

Provided herein are atomic layer deposition (ALD) methods of depositing cobalt in a feature. The methods involve two-step surface treatments during an ALD cycle, with one step involving the reaction of a co-reactant gas with an adsorbed cobalt precursor and the other step involving a growth-inhibiting reactant gas on the cobalt surface. The growth-inhibiting reactant gas significantly lowers cobalt growth rate, producing a highly conformal cobalt film. The described ALD processes enable improved controllability in film nucleation, step coverage, and morphology by the separate surface treatment and low process temperature. The methods are applicable to a variety of feature fill applications including the fabrication of metal gate/contact fill in front end of line (FEOL) processes as well as via/line fill in back end of line (BEOL) processes.

Methods and apparatus for forming smooth and conformal cobalt film by atomic layer deposition

The effect of dimethylglyoxime on Co electrodeposition was investigated with cyclic voltammetry, chronopotentiometry, quartz microbalance as well as electrochemical impedance. A potential dependent suppression effect was observed at low potential with a breakdown of the suppression at high potential, resulting in a hysteresis in CV. The addition of dimethylglyoxime not only causes a fast and strong suppression in potential transients but also modifies the impedance spectra. Additional capacitive loops and inductance loops emerged depending on the applied potential, suggesting a competitive adsorption between different surface adsorbed intermediates. A relaxation of suppression effect was observed in absence of agitation and a strong suppression was re-established upon agitation. A reverse relation between Co deposition rate and rotation rate was observed when the rotation rate is below a critical value, providing a path to enable the preferential deposition at the bottom of a small damascene feature.

https://iopscience.iop.org/article/10.1149/2.1111613jes/pdf

Electrodeposition of Cobalt for Interconnect Application: Effect of Dimethylglyoxime

Alternate metallization schemes for copper interconnect using selective CVD Co capping at the 22nm technology node are investigated. Control splits fabricated with PVD Ta(N) barrier/liner layers and CuMn alloy seedlayers are compared against interconnects fabricated using a PVD TaN barrier/CVD Co liner scheme with selective CVD Co capping. Secondary ion mass spectroscopy (SIMS) studies of PVD TaN barrier/CVD Co liner structures indicates that top-surface segregation of the Mn-dopant in alloy seedlayers is suppressed in the presence of the CVD Co Liner. Alternate metal capping in the form of selective CVD Co layers is evaluated in combination with CVD Co liners. Good electrical yields are obtained in-line with the Co liner/Co cap scheme. The PVD TaN/Co-Liner/Selective CVD Co cap combination is seen to have greatly enhanced electromigration performance over PVD Ta(N)/PVD CuMn controls, with T50 fail times for the former being ~100x longer than the controls. Kinetics studies of the CVD Co liner/selective Co cap samples show electromigration activation energies of 1.7 eV, a substantial enhancement over the 1.0 eV obtained for the PVD Ta(N)/CuMn controls.

Electromigration comparison of selective CVD cobalt capping with PVD Ta(N) and CVD cobalt liners on 22nm-groundrule dual-damascene Cu interconnects

Fundamental material interactions as pertinent to nano-scale copper interconnects were studied for CVD Co with a variety of micro-analytical techniques. Native Co oxide grew rapidly within a few hours (XPS). Incorporation of oxygen and carbon in the CVD Co films (by AES and SIMS) depended on underlying materials, such as Ta, TaN, or Ru. Copper film texture (by XRD) and agglomeration resistance (by AFM) showed correlations with amounts of in-film oxygen/carbon. Cobalt diffused through copper at normal processing temperatures (by SIMS). CVD Co demonstrated diffusion barrier performance to Cu (by Triangular Voltage Sweep, TVS), but not to O 2 . CVD Co was applied to 32 nm/22 nm damascene Cu interconnect fabrication in a scheme defined by the material studies. Lower post-CMP defect density and longer electromigration lifetimes were obtained.

CVD Co and its application to Cu damascene interconnections

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CVD Co and its application to Cu damascene interconnections