Influence of electrolysis variables on the passivation time of copper anodes in copper electrorefining

Sędzimir, J.; Gumowska, W.

doi:10.1016/0304-386x(90)90087-i

Cited by 20 publications

(7 citation statements)

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“…52 The stability of supersaturated liquid and of salt layer is critically dependent on composition and on intensity of processes, especially on the mutual relations of the electrochemical dissolution and transport rates. [53][54][55] The remarkable feature of plots shown in Fig. 1 and 2 is the presence of current minima ͑dips͒ on the anodic side of the active/passive transition peak.…”

Section: Resultsmentioning

confidence: 94%

Kramers-Kronig Transforms as Validation of Electrochemical Immittance Data Near Discontinuity

Sadkowski

Dolata

Diard

2004

J. Electrochem. Soc.

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International audienceImmittance data was recorded for copper rotating disk in concentrated copper sulphate/sulphuric acid electrolyte, and its evolution under potential control (PC) was analyzed starting from the active state at rest potential, through active/passive transition up to the stable passivity. In the potential range corresponding to the passivity under PC, the transition was observed from the nonminimum phase (nmp)-type of immittance to the minimum phase (mp) one which corresponded to Hopf bifurcation under current control. This transition was manifested by a resonance-like peak on the amplitude characteristic and the phase change from apparently discontinuous as displayed in [–180°, +180°] range (nonminimum) to the continuous (minimum) one. In complex coordinates this was featured by scattered impedance points. Validation by Kramers-Kronig (KK) transformation of nmp-type immittance data failed for impedance representation used in transformation but was successful for admittance representation as the latter was the form actually recorded under PC. This finding validates both nmp and mp immittance data in agreement with earlier suggestions of other authors. [See, Gabrielli et al., in Electrochemical Impedance: Analysis and Interpretation, p. 140, ASTM, Philadelphia, PA (1993).] Transition from mnp to mp type of electrode dynamics can be attributed to appearance of conduction channels representing local depassivation of the electrode

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Section: Resultsmentioning

confidence: 94%

Kramers-Kronig Transforms as Validation of Electrochemical Immittance Data Near Discontinuity

Sadkowski

Dolata

Diard

2004

J. Electrochem. Soc.

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“…25 Copper anodes containing phosphorus are known to prevent Cu I release into the plating bath by either favoring the direct two-electron copper reduction reaction or by trapping Cu I in black films generated on the anode. 17,29,30 It was also shown in the model that the inductive loop was directly associated with the surface coverage of the Cu I -accelerator complex, which increases as its concentration in the bath increases, independent of the additive ͑PEG, MPSA, or SPS͒ concentrations in the bath. 12 Moreover, an increase in the size of the inductive loop was observed when either MPSA or SPS concentration was increased in a freshly made plating bath.…”

Section: D14mentioning

confidence: 94%

A Model for Copper Deposition in the Damascene Process

Gabrielli

Moçotéguy

Perrot

et al. 2007

J. Electrochem. Soc.

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Previously, a model of copper deposition in the damascene process was proposed that takes into account the existence of a copper-accelerator complex as well as the competitive adsorption of an inhibitor and an accelerator. The model was verified experimentally by electrochemical impedance spectroscopy and dc voltammetry measurements on fresh solutions of a superfilling, copper deposition plating bath. In this paper, the same model was applied to plating baths during copper deposition where aging and possible relaxation of the bath back to a steady state can occur. The model can provide insight into interpreting the impedance spectra during and after copper deposition. Changes in the Cu-accelerator complex in the bulk solution and the surface coverage of this complex were followed using a parameter based on the low-frequency inductive loop of the electrochemical impedance spectra. Results indicate that the impedance spectroscopy measurements are mainly sensitive to Cu-accelerator complex formation and destruction.The damascene process for fabrication of copper on-chip metal interconnects requires electrodeposition into trenches or vias with width dimensions on the order of 130 nm or lower. To obtain voidfree deposits, superconformal deposition, or superfilling, is necessary. These terms refer to the occurrence of more rapid electrodeposition in the bottom of a trench or via than toward its entrance. Copper electroplating baths usually contain a mixture of H 2 SO 4 and CuSO 4 in concentrations close to 1.8 and 0.25 M, respectively, to which chloride ions are added in the range of 1 to 2 mM. However, superfilling is only obtained in the presence of a certain combination of additives in the electroplating bath, 1,2 including brighteners/ accelerators, carriers/suppressors, and levellers. Brighteners are usually propane sulfonic acid derivatives, either MPSA

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“…In this process, pure copper is produced and also, valuable impurities are removed from the impure copper as anodic slime [1,2,4]. Copper anodes with a purity of 98.5 to 99.5% is used loss because the anode has to be removed and melted again [5][6][7][8][9][10][11][12][13].…”

Section: Introductionmentioning

confidence: 99%

Modeling and Optimization of Charge Materials Ranges in Converter Furnace with Enhanced Passivation Time in Copper Electrorefining Process: A Mixture Design Approach

Feizabad

Khayati

Hernashki

et al. 2021

IJE

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In this study, the design of experiments is used to study and model the time of passivation in copper electrorefining as a function of the charge of melting furnace through the preparation of copper casting anodes. As a result of optimization for the proposed optimized anodes, the charge percent values of concentrate (Co), refinery scrap (RS), and non-refinery scrap (NRS) were proposed equals to 69.1, 0.574 and 30.32 (wt.%), respectively. Experimental data confirmed the enhanced passivation time of the proposed anode was 6520 s. Also, it was observed that the molar ratio of As/(Bi+Sb) and Ag/(Se+Te) are the key factors in passivation time. Finally, the relation of passivation time (seconds) with the charge of melting furnace is proposed as : t (s)= -3728.98 × Co + 4640.00 × RS + 3141.00 × NRS + 17763.27 × Co × RS + 25547.65 × Co × NRS -1758.00 × RS × NRS. Moreover, adding of As ingot in casting anodes as a dose dependent of non-refinery scrap portion in the input charge of the melting unit can effectively prolong the time of passivation.

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Influence of electrolysis variables on the passivation time of copper anodes in copper electrorefining

Cited by 20 publications

References 1 publication

Kramers-Kronig Transforms as Validation of Electrochemical Immittance Data Near Discontinuity

Kramers-Kronig Transforms as Validation of Electrochemical Immittance Data Near Discontinuity

A Model for Copper Deposition in the Damascene Process

Modeling and Optimization of Charge Materials Ranges in Converter Furnace with Enhanced Passivation Time in Copper Electrorefining Process: A Mixture Design Approach

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